Day: January 6, 2021

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.144690-92-6, molecula formula is Triphenyl methyl olmesartan, below Introduce a new synthetic route., 144690-92-6

To 3L reaction flask 165.3g above prepared 1 – [[[2- (triphenylmethyl) -2H- tetrazole-5-yl] biphenyl-4-yl] methyl] -2- propyl-4- (1-hydroxy-1-methylethyl) imidazole-5-carboxylic acid (5-methyl-2-oxo-1,3-dioxolen-4-yl) methyl ester ( compound ) and 1.90L70% acetic acid, mechanical stirring, heated to 50 , the reaction 2.5h, an ice bath was added 1.1L of water was stirred.Filtration, the filtrate with 300ml * 3 times extracted with methylene chloride, the methylene chloride phase 150mL ¡Á 5 times with 5% acetic acid solution was washed with acetic acid solution and extracted with 250ml of dichloromethane, and the combined organic phases.The solvent was distilled off under reduced pressure, the residue was added 380mL of ethyl acetate was heated with stirring and cooling to precipitate a solid.Suction filtered, the filter cake was dried in vacuo to give a white solid product to 89.6 g, weight yield was 77.8%.To a 1L reaction flask above 85g crude product olmesartan medoxomil, 420ml of tetrahydrofuran was heated at reflux, was added 360ml of ethyl acetate, the ice bath was stirred for crystallization.Filtration cake blast drying to constant weight to give the product as a white solid 74.8g, a yield of 83.5% by weight., 144690-92-6

Elementary reactions that involve the simultaneous collision of more than three molecules are highly improbable and have never been observed experimentally.

Reference£º
Patent; Bengbu Tu Shan Fengyuan Pharmaceutical Co., Ltd.; Ma, Qisheng; Li, Baoqin; Sun, Peng; (18 pag.)CN105418593; (2016); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.Triphenyl methyl olmesartan, cas is 144690-92-6. Here is a downstream synthesis route of the compound 144690-92-6, 144690-92-6

To the three-necked flask were added with 38 ml of ethyl acetate, 45 g of 6.4% dilute hydrochloric acid, 25 g of trityl olmesartan medoxomil was added with stirring. Stir in water bath, control the temperature 15 to 20 C, stirring about 4 hours, TLC plate detection point of raw material disappeared,That is, it is judged that the deprotection reaction is completed.Cooled to room temperature, 115 ml * 5 toluene was added to wash, the aqueous layer was added with 135 ml of acetone, potassium bicarbonate aqueous solution adjusted P=4.0, control temperature 15 ¡À 5 C Stir for 2 hours, Filtered and dried to give 16.0 g of olmesartan medoxomil in a yield of 90.2%. HPLC analysis: purity 98.75%, impurity a (olmesartan acid) 0.71%, individual impurities less than 0.10%

144690-92-6 is used more and more widely, we look forward to future research findings about Triphenyl methyl olmesartan

Reference£º
Patent; Zhejiang Huahai Pharmaceutical Co., Ltd,; Huang, Xiangliang; Zhang, LI; Hua, yuanyuan; Wu, Yong De; (7 pag.)CN102584804; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.144690-92-6. A new synthetic method of this compound is introduced below.

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%

With the complex challenges of chemical substances, we look forward to future research findings about Triphenyl methyl olmesartan

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

37830-90-3, A balanced equation for a chemical reaction indicates what is reacting and what is produced, but it reveals nothing about how the reaction actually takes place. The reaction mechanism is the process, or pathway, by which a reaction occurs.37830-90-3. An updated downstream synthesis route of 37830-90-3 as follows.

PREPARATION 2 Preparation of 4-bromomethyl-5-methyl-1,3-dioxole-2-one According to the method described in Liebigs. Ann. Chem., 1977, 27-32 4,5-dimethyl-1,3-dioxole-2-one (500 mg, 4.38 mmol) and N-bromosuccinimide (0.78 g, 4.38 mmol) were heated under reflux in dry carbon tetrachloride in the presence of alpha-alpha’-azobisisobutyronitrile (7.5 mg) for 20 minutes. The reaction mixture was concentrated under reduced pressure to half the volume, and the precipitated solid was filtered by suction. After removing the solvent from the filtrate, the residue was analyzed by gas chromatography. The obtained mixture (792 mg), contained 70percent of the desired title compound and used for the subsequent reactions.

A chemical reaction often occurs in steps, although it may not always be obvious to an observer.

Reference£º
Patent; Sawai Pharmaceutical Co., Ltd.; US5006548; (1991); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

37830-90-3, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.37830-90-3. A new synthetic method of this compound is introduced below.

(1) 4-Bromomethyl-5-methyl-1,3-dioxolen-2-one [compound of formula (III) in which R is methyl and X is bromine] 3.42 g of 4,5-dimethyl-1,3-dioxolen-2-one [compound of formula (III’) in which R is methyl, prepared in accordance with the procedure described in Tetrahedron Letters, pages 1701-1704, (1972)] was dissolved in 150 ml of carbon tetrachloride. To the solution were added 5.34 g of N-bromosuccinimide and a catalytic amount of alpha,alpha’-azobisisobutyronitrile. The mixture was heated under reflux for 15 minutes. The reaction mixture was cooled with ice, and the insoluble materials were removed by filtration. The filtrate was concentrated under reduced pressure to give a syrupy residue. The residue was distilled under reduced pressure, and a fraction having a boiling point of 115¡ã to 120¡ã C./5 mmHg was recovered. Thus, 4.2 g (yield 73percent) of the captioned compound having the following properties was obtained as a colorless liquid. Elemental analysis for C5 H5 BrO3: IR (neat) nu(cm-1): near 18 25 (carbonyl). NMR (CCl4) delta(ppm): 2.10 (3H, –CH3, s), 4.10 (2H, –CH2 Br, s).

Elementary reactions that involve the simultaneous collision of more than three molecules are highly improbable and have never been observed experimentally.

Reference£º
Patent; Kanebo Ltd.; US4448769; (1984); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, The molecularity is the number of molecules that collide during that step in the mechanism. If only a single reactant molecule in an elementary reaction, that step is designated as unimolecular; if there are two reactant molecules, it is bimolecular.80841-78-7. A new synthetic method of this compound is introduced below.

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%.

The chemical industry reduces the impact on the environment during synthesis, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, , I believe this compound will play a more active role in future production and life.

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

An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.4,5-Dimethyl-1,3-dioxol-2-one, cas is 37830-90-3. Here is a downstream synthesis route of the compound 37830-90-3, 37830-90-3

A mixture of 4,5-dimethyl-1,3-dioxol-2-one (1.0 g, 8.8 mmol), benzoylperoxide (60 mg, 0.25 mmol) and N-bromosuccinimide (1.6 g, 9.0 mmol) in carbon tetrachloride (10 mL) was heated at reflux for 2 h. The solid was removed from the reaction mixture by filtration. The mother liquid was washed with sat. NaHCO3 and brine, dried over MgSO4 and concentrated. The crude product, 4-(bromomethyl)-5-methyl-1,3-dioxol-2-one, was obtained as a yellow oil (1.7 g) and was used without further purification in the next step.

A chemical reaction often occurs in steps, although it may not always be obvious to an observer.

Reference£º
Patent; Martinsson, Jessica; Faernegardh, Katarina; Joensson, Mattias; Ringom, Rune; US2015/25068; (2015); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Rate laws may be derived directly from the chemical equations for elementary reactions. This is not the case, however, for ordinary chemical reactions.144690-92-6, molecula formula is Triphenyl methyl olmesartan, below Introduce a new synthetic route., 144690-92-6

The reaction flask was charged with 400 g of compound VII (0.50 mol) and 70% aqueous acetic acid solution of 3200 ml, Reaction was carried out at 50 C for 2 hours. After the completion of the reaction, the solvent was concentrated and concentrated, and ammonia was added to the residue.PH = 7, extracted with 1400 ml of ethyl acetate, the ethyl acetate layer was washed with water, and finally with anhydrous sodium sulfateDried; filtered, the filtrate was concentrated to dryness and the residue was recrystallized from ethanol to give the compound I pure product 256.1G, yield: 91.79%.

With the synthetic route has been constantly updated, we look forward to future research findings about Triphenyl methyl olmesartan,belong Dioxole compound

Reference£º
Patent; Hunan Ouya biological Co. Ltd.; Lin, kaizhao; (19 pag.)CN103304550; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

An elementary termolecular reaction involves the simultaneous collision of three atoms, molecules, or ions.Triphenyl methyl olmesartan, cas is 144690-92-6. Here is a downstream synthesis route of the compound 144690-92-6, 144690-92-6

Take 40g of compound 5, Add 80mL of methanol, 330 mL of ethyl acetate, Warmed to 45 , After 8 hours of reaction, Add 860mL water, Insoluble matter was removed by filtration, The filtrate was concentrated, In oily liquid, Acetonitrile, Stirred under a solid precipitation, filter, Washed with ethanol, 23.2 g of white solid was obtained, The yield was 83.1% The HPLC purity was 99.2%.

The chemical industry reduces the impact on the environment during synthesis, Triphenyl methyl olmesartan, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Disha Pharmaceutical Group Co., Ltd.; Zhang Zhaoxing; Zhang Hongqiang; Qin Litai; Li Wei; Li Zongwen; Xia Haijian; (6 pag.)CN103012382; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem