Day: February 22, 2021

80841-78-7,is a common compound. C5H5ClO3In an article, once mentioned the new application about 80841-78-7.

Example 5: The reaction part was charged with ethyl 4- (1-hydroxy-1-methylethyl) -2-propyl-1- {4- [2- (trityltetrazol-5-yl) phenyl] 22 g of 5-carboxylate (Formula 4), 3.1 g of sodium hydroxide and 90 mL of ethanol were added and the mixture was stirred at 20 to 25 C for 4 to 5 hours. When the reaction was completed, the reaction solution was concentrated. To the residue were added 50 mL of ethyl acetate and 50 mL of purified water. The mixture was stirred for 1 hour and then layered. The separated organic layer was washed twice with an aqueous solution containing 30 g of salt and 170 mL of purified water. 1 g of activated carbon and 20 g of anhydrous sodium sulfate were added to the organic layer, followed by stirring for 30 minutes to 1 hour, followed by filtration Respectively. After the filtrate was concentrated under reduced pressure, 50 mL of N, N-dimethylacetamide was added to the residue, the temperature was adjusted to 5 to 10 DEG C 4 g of potassium carbonate was added and 6.2 g of 4- (chloromethyl) -5-methyl-1,3-dioxol-2-one (Formula 6) was dissolved in N, N-dimethylacetamide 6 ML was added dropwise, and the mixture was reacted at 45 to 50 C for 4 hours with stirring. When the reaction is completed, the reaction solution is cooled to 20 to 25 After cooling, 220 mL of ethyl acetate, 30 g of salt and 170 mL of purified water were added successively. The organic layer was separated And then washed once more with an aqueous solution containing 30 g of salt and 170 mL of purified water. The organic layer was washed with 1 g of activated carbon, 20 g of sodium was added and stirred for 30 minutes to 1 hour, followed by filtration. The filtrate was concentrated under reduced pressure, and then acetone 100 mL of i-tril was added, and the mixture was stirred at 50 to 55 C for 1 hour. The crystals were cooled to 0 to 5 [deg.] C and stirred for 2 hours. Followed by washing with 50 mL of isopropyl alcohol, followed by drying to obtain 21.6 g (yield: 88%) of tritylolemecanemethoxysilane (formula 1a) Purity 99.97%) was obtained

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Reference£º
Patent; DONGBANG FTL CO., LTD; Song, Tae Hong; Jung, Hun Suk; Jang, Do Yeon; Moon, Chung Sun; Jung, Hee Jung; (18 pag.)KR101526249; (2015); B1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In an article, published in an article,once mentioned the application of 80841-78-7,molecular formula is , is a conventional compound. this article was the specific content is as follows. 80841-78-7

Example 5; Preparation of trityl olmesartan medoxomilTo dimethyl sulphoxide (800 ml), sodium hydroxide powder (50 gms) was added under nitrogen atmosphere and stirred at 20-250C for 10 minutes. To this, 4-( 1 -hydroxy- 1- methylethyl)-2-propyl-imidazole-5-ethyl carboxylate (100 gms) was added at 20-250C. 5- (4′-bromomethyl-biphenyl)-2-yl-1 -trityl tetrazole (270 gms) was added slowly at 20-250C, and the reaction mass was stirred at 20-250C for 12 hours. Further 10% sodium hydroxide solution (100 ml) was added to the reaction mass at 20-250C. The temperature of the reaction mass was raised to 40-450C, the contents stirred at 40-450C for 2 hours and 5- methyl-2-oxo-1 ,3-dioxane-4-yl)methyl chloride (160 gms) was added slowly at 45-5O0C over a period of 45 minutes. The contents were stirred at 45-5O0C for 2 hours. The reaction mass was then cooled to 0-50C, stirred for 1 hour at 0-50C, filtered and slurried in water (1.0 It) at 40-450C for 1 hour, filtered at 4O0C and dried at 4O0C. To the dried material, ethyl acetate (2.5 It) was added, heated to 50-550C for complete dissolution, ethyl acetate was distilled off to 1.0 It stage under vacuum at 45-5O0C. The contents were cooled to 0-50C, stirred at 0-50C for 3 hours, filtered, washed with chilled methanol (100 ml) and dried under vacuum at 40-450C to give 250 gms of the title compound. Purity by HPLC : > 99%

The proportionality constant is the rate constant for the particular unimolecular reaction. the reaction rate is directly proportional to the concentration of the reactant. I hope my blog about 80841-78-7 is helpful to your research. 80841-78-7

Reference£º
Patent; CIPLA LIMITED; CURTIS, Philip, Anthony; WO2008/43996; (2008); A2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6,Let¡¯s face it, organic chemistry can seem difficult to learn. Especially from a beginner¡¯s point of view. Like C48H44N6O6,introducing its new discovery.

78(b) (5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate 75 ml of water were added to a suspension of 29.3 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (a) above] in 225 ml of acetic acid, and the resulting mixture was stirred at 60 C. for 1.5 hours. At the end of this time, 75 ml of water were added to the mixture, which was then cooled. Precipitated trityl alcohol was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure. Toluene was added to the residue, and the mixture was again concentrated by evaporation under reduced pressure, to remove the remaining water and acetic acid. The residue was crystallized in ethyl acetate, to give 16.6 g of the title compound as crystals, melting at 177-180 C. (with decomposition). The Nuclear Magnetic Resonance Spectrum of this compound was identical with that of the compound obtained as described in Example 61(b).

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Reference£º
Patent; Sankyo Company, Limited; US5616599; (1997); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6,is a common compound. C48H44N6O6.In an article, once mentioned the new application about 144690-92-6.

Trityl olmesartan medoxomil (250 g, 310 mmol) (97.3 % area) is dissolved in THF (1560 ml) and 48 % aqueous hydrobromic acid (70.6 ml, 625 mmol) is added slowly. The mixture is stirred for at 25 C. After 1 hour the precipitate forms. The mixture is stirred for 1 additional hour at 25 C, then cooled to -5 C and stirred for 1.5 hours at -5 C. The precipitate is filtered. 940 ml of THF is added to the precipitate and the mixture is stirred for 1 h at 25 C and then 1 hour at -5 C. Then precipitate is filtered off and washed with cold THF (150 ml). It is then dissolved in a mixture of water (875 ml) and acetone (440 ml). To a clear solution 5 % aqueous solution of NaHCO3 is added to raise pH to 5.15. The mixture is stirred for 1 hour at room temperature and 1 hour at 0 C. The precipitate is filtered, washed with water and then recrystallized from a mixture of acetonitrile (280 ml) and water (70 ml) to give 124.5 g of olmesartan medoxomil (99.68 % area)

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Reference£º
Patent; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 144690-92-6

Example 1; Preparation of olmesartan medoxomilTo dimethyl acetamide (300 ml) was added 4-(1-hydroxy-1-methylethyl)-2-propyl imidazol- 5-carboxylic acid ethyl ester (50 gms) and powdered sodium hydroxide (26 gms). To this, 4-[2-(trityltetrazol-5-yl)phenyl]benzyl bromide (135 gms) was charged at 45-500C. The contents were stirred for 5 hours at 45-500C. Diisopropylethyl amine (100 ml) was charged to the reaction mass at 40-450C. A solution of 5-methyl-2-oxo-1 , 3-dioxane-4-yl)methyl chloride (80 gms) diluted with dimethyl acetamide (160 ml) was slowly added to the reaction mass at 40-450C over a period of 1 hour. The contents were heated to 60-650C and maintained for 4 hours. The reaction mass was then cooled to 30-350C and neutralized with concentrated hydrochloride acid. The reaction mass was filtered to remove inorganic impurities, charcoalized using charcoal (10 gms) andstirred for 30 minutes at 40-450C. The reaction mass was filtered over hyflo. The clear filtrate was acidified with hydrochloric acid (100 ml) slowly at 25-30C. The contents were stirred at 60C for 1 hour. The reaction mass was chilled to 0-5C and filtered to remove tritanol. The reaction mass was concentrated under reduced pressure. The residue was quenched with water (500ml), neutralized with base and extracted in dichloromethane (500 ml). The clear dichloromethane extract was then concentrated under reduced pressure and stripped off with acetone. The residue thus obtained was isolated from acetone (250 ml) to give 55 gms of the title compound. Chromatographic purity- > 99%; Example 2Preparation of olmesartan medoxomilTo dimethyl acetamide (600 ml) was added 4-(1-hydroxy-1-methylethyl)-2-propyl imidazol- 5-carboxylic acid ethyl ester (100 gms) and powdered potassium hydroxide (50 gms). To this was charged 4-[2-(trityltetrazol-5-yl)phenyl]benzyl bromide (270 gms) at 45-50C. The contents were stirred for 5 hours at 45-50C. Diisopropylethyl amine (200 ml) was charged to the reaction mass at 40-450C. To this was slowly added a solution of 5-methyl-2-oxo- 1 ,3-dioxane-4-yl)methyl chloride (160 gms) diluted with dimethyl acetamide (320 ml) at 40- 45C over a period of 1 hour. The contents were heated to 60-650C and maintained for 4 hours. The reaction mass was then cooled to 30-350C and was neutralized with concentrated hydrochloride acid. The reaction mass was filtered to remove inorganic impurities. The reaction mass was charcoalized using charcoal (20 gms) and was stirred for 30 minutes at 40-450C. The reaction mass was filtered over hyflo. The clear filtrate was acidified with hydrochloric acid (200 ml) slowly at 25-300C. The contents were stirred at 60C for 1 hour. The reaction mass was chilled to 0-50C and was filtered to remove tritanol. The reaction mass was concentrated under reduced pressure. The residue was quenched with water (1000 ml), neutralized with base and extracted in dichloromethane (1000 ml). The clear dichloromethane extract was then concentrated under reduced pressure, stripped off with acetone. The residue thus obtained was isolated from the acetone (500 ml) to give 110 gms of the title compound. Chromatogrphic purity- > 99%; Example 3Preparation of olmesartan medoxomilTo dimethyl acetamide (800 ml) was added 4-(1-hydroxy-1-methylethyl)-2-propyl imidazol- 5-carboxylic acid ethyl ester (100 gms) and powdered potassium carbonate (200 gms). To this was charged 4-[2-(trityltetrazol-5-yl)phenyl]benzyl bromide (300 gms) at 45-50C. The contents were stirred for 8-10 hours at 45-50C. The insolubles were filtered. The contents were cooled to 5-100C. Potassium tertiary butoxide (100 gms) was charged at a temperature below 45C. The reaction was maintained at 40-450C for 3 hrs. To this was slowly added 5-methyl-2-oxo-1 ,3-dioxane-4-yl) methyl chloride at 40-450C over a period of 1 hour. The contents were heated to 60-650C and maintained for 4 hours. The reaction mass was then cooled to 30-350C and was neutralized with concentrated hydrochloride acid. The reaction mass was filtered to remove inorganics. The reaction mass was charcoalized using charcoal (10 gms) and was stirred for 30 minutes at 40-450C. The reaction mass was filtered over hyflo. The clear filtrate was acidified with hydrochloric acid (100 ml) slowly at 25-30C. The contents were stirred at 60C for 1 hour. The reaction mass was chilled to 0-5C and was filtered to remove tritanol. The reaction mass was concentrated under reduced pressure. The residue was quenched with water (500 ml), neutralized with base and extracted in dichloromethane (500 ml).The clear dichloromethane extract was then concentrated under reduced pressure, stripped off with acetone. The residue thus obtained was isolated from the acetone (250 ml) to give 55 gms of the title compound. Chromatogrphic purity- > 99%

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Reference£º
Patent; CIPLA LIMITED; CURTIS, Philip, Anthony; WO2008/43996; (2008); A2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Chemistry is the experimental and theoretical study of materials on their properties at both the macroscopic and microscopic levels. 80841-78-7. In a patent£¬Which mentioned a new discovery about 80841-78-7, molcular formula is C5H5ClO3, introducing its new discovery.

Step B, go to the reaction solution of compound (II) obtained in Step A with stirring,Add 6.27kg of anhydrous sodium carbonate powder and 2.01kg of iodine, replace the air with nitrogen,The nitrogen pressure in the kettle is ?0.01Mpa, the control temperature is 50 ¡À 2 ,15.05 kg of compound (IV) was added dropwise at a constant pressure, and the addition was completed within 40 to 60 minutes.After the reaction was held for 1 hour, the reaction mixture was reduced to below 10 C.Extract with conventional solvents in an extraction kettle, wash with water, and separate the layers.The organic phase was distilled under reduced pressure to recover the solvent, crystallized, centrifuged,After drying, 54.88 kg of the crude compound (I) was obtained.Step C: Add 192.08 kg of ethyl acetate to the 500L refining kettle, start stirring,Add 54.88 kg of crude compound (I) obtained in step B, close the feed port,Keep the pressure ?0.01MPa after replacing air with nitrogen,The temperature was raised to 75 C and dissolved for 25 minutes until it was clear. The filtrate was filtered and the temperature was reduced to 2.5 C.Centrifuge, put the filter cake into the double cone dryer,Under reduced pressure, a small flow of nitrogen was passed in for replacement three times, and the drying temperature was controlled to 40-50 C.Vacuum degree ?-0.09MPa, after drying for 1 hour,Increase the drying temperature to 50 60 and continue drying for 3 hours.After cooling down, 53.60 kg of compound (1) was obtained, and the HPLC content was 99.87%.Compound (III) had a residual content of 0.06%.

I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 80841-78-7, help many people in the next few years.C5H5ClO3

Reference£º
Patent; Shandong Xinhua Pharmaceutical Co., Ltd.; Zhu Lianbo; Wu Hui; Dou Guohua; (6 pag.)CN110590758; (2019); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Chemistry is the experimental and theoretical study of materials on their properties at both the macroscopic and microscopic levels. 37830-90-3. In a patent£¬Which mentioned a new discovery about 37830-90-3, molcular formula is C5H6O3, introducing its new discovery.

Compound 20 was prepared following the steps disclosed in the literature (Sakamoto er a/., Chem. Pharm. Bull, 1984, 32, 2241).

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Reference£º
Patent; ANCHEN LABORATORIES, INC; WO2009/118580; (2009); A2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6,Let¡¯s face it, organic chemistry can seem difficult to learn. Especially from a beginner¡¯s point of view. Like C48H44N6O6,introducing its new discovery.

To TOLM (75 g) were successively added acetic acid_water=1:1 (330 mL, 4.4 vol) and concentrated sulfuric acid (5.4 mL, 1.08 eq). The obtained mixture was stirred at 25C – 30C for 1 hr. Using TLC (thin layer chromatography) (TLC eluent: 10% methanol/methylene chloride, detection method: UV), complete disappearance of TOLM was confirmed. [0309] The reaction mixture was filtered and insoluble trityl alcohol was removed. The aqueous layer was adjusted to pH 2 – 3 by adding 25% aqueous sodium carbonate solution (initial pH of the reaction mixture was 4 – 4.5). The reaction mixture was stirred for 5 min, methylene chloride (225 mL, 3 vol) was added thereto, and the mixture was stirred for 5 min. Stirring was stopped, and the mixture was stood and partitioned. The aqueous layer was extracted with methylene chloride (2×225 mL, 2×3 vol), the extracts were combined with the organic layer, deionized water (375 mL, 5vol) was added, and the mixture was stirred for 5 min. Stirring was stopped, and the mixture was stood for 5 min and partitioned. To the organic layer was added saturated brine (375 mL, 5 vol), and the mixture was stirred for 5 min, left standing and partitioned. The organic layer was concentrated under reduced pressure at 40C – 45C to give crude OLM MDX (49 g, 93%) as a pale-yellow solid.To the crude OLM MDX (49 g, 1 eq) obtained in the above-mentioned (7) was added acetone (735 mL, 15 vol), and the mixture was stirred at 55C – 60C for 10 min. Furthermore, the reaction mixture was stirred at the same temperature for 15 min, and acetone was evaporated under normal pressure. Heating was stopped when a solid was precipitated, and the mixture was cooled to 25C – 30C. The precipitated solid was collected by filtration and dried with suction for 30 min to give OLM MDX (41 g, 83%). [0311] To the OLM MDX obtained above was added isopropyl alcohol (164 mL, 4 vol), and the mixture was heated to 55C – 60C, and stirred at 55C – 60C for 1 hr. Heating was stopped and the mixture was gradually cooled to 25C – 30C, and stirred at 25C – 30C for 30 min. The precipitated solid was filtered and dried with suction to give OLM MDX (41 g, 100%). [0312] The OLM MDX (41 g) obtained above and acetone (about 1 L) were heated to 55C – 60C, and stirred at 55C – 60C for 25 min. Acetone was evaporated under normal pressure until the mixture became cloudy, and the mixture was gradually cooled to 25C – 30C. The precipitated solid was collected by filtration and dried with suction for 30 min to give OLM MDX (34 g, 83%). The HPLC purity of the obtained OLM MDX was 99.66%. [0313] The OLM MDX (44 g) obtained above was dissolved in acetone (about 1.2 L), and the mixture was stirred at 55C-60C for 10 min. Acetone was evaporated under normal pressure until the solution became cloudy, and the solution was gradually cooled to 25C – 30C. The precipitated solid was collected by filtration, dried with suction for 30 min, blast dried for 1 hr, and further blast dried at 40C – 45C for 5 hr to give OLM MDX (36 g) as a white solid. The HPLC purity of the obtained OLM MDX was 99.8%.

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Reference£º
Patent; API Corporation; SEKI, Masahiko; EP2891650; (2015); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

In an article, published in an article,once mentioned the application of 144690-92-6,molecular formula is , is a conventional compound. this article was the specific content is as follows. 144690-92-6

To 12.0g (15 mmol) of tritylolmesartan medoxomil prepared according to examples 1 or 2 69 ml of ethyl acetate was added and after that 12 ml of methanol and 2.67 ml (32 mmol) of conc. HCl were added. The mixture was stirred at room temperature for 2h and then the mixture was cooled to below 2C. To the cooled mixture 71 ml of 1% NH3 was slowly added to adjust pH to 4.93. The phases were separated and water phase was reextracted with 20 ml of ethyl acetate. Collected organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure to approximately 15g of oily residue. To this residue 15 ml of ethyl acetate were added and the mixture was cooled to 20 C and stirred at this temperature for 2h, and then cooled under 0C and stirred at this temperature for 1hour. The product was filtered off and washed with 5 ml of fresh ethyl acetate and dried. Yield: 7.55 g (90%). HPLC: 99.81 % of the product, all individual impurities under 0.10%.

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Reference£º
Patent; Krka Tovarna Zdravil, D.D., Novo Mesto; EP2334668; (2011); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6,Children learn through play, and they learn more than adults might expect. Science experiments are a great way to spark their curiosity, get their minds active, and encourage them to do something that doesn¡¯t involve a screen. C48H44N6O6,introducing its new discovery.

Trityl olmesartan medoxomil (8 g, 10 mmol) is dissolved in THF (25 ml) and diethyl ether (25 ml) and 48 % aqueous hydrobromic acid (3.5 ml, 30 mmol) is added. The mixture is stirred for 1 hour at room temperature and then 1 hour at 0 C. The precipitate is filtered, washed with cold THF (20 ml) and dried overnight in vacuum at room temperature to give 5.0 g of olmesartan medoxomil hydrobromide Form B

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Reference£º
Patent; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem