Dioxole related

144690-92-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Triphenyl methyl olmesartan, cas is 144690-92-6,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5

The chemical industry reduces the impact on the environment during synthesis,144690-92-6,Triphenyl methyl olmesartan,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, cas is 80841-78-7,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

Example 2; 36.0 g (50.3 mmol) ethyl 4-(l -hydroxy- 1-methy lethyl)-2-propy 1-1- {4-[2-(trityltetrazol-5-y I)- phenyl]phenyl} -methyl imidazole-5-carboxylate (Va) and 3.0 g (75.4 mmol) of NaOH were suspended in 413 ml dimethylacetamide. The suspension was then stirred at room temperature for 20 h and after that 6.9 g (50.3 mmol) of K2CO3, were added. The mixture was cooled to 00C and solution of 15.4 g (70.4 mmol) 4-chloromethyl-5-methyl-2-oxo-l,3- dioxolene in 39 ml of dimethylacetamide were slowly added. The mixture was slowly heated to 500C and stirred at this temperature for 2 h. After esterification was completed, the mixture was cooled to 10 0C and poured into a mixture of 625 ml of ethyl acetate and 625 ml of 10 % NaCl, and stirred at 25 0C for 15 min. The phases were separated and organic phase was washed 2chi with 500 ml of 10 % NaCl, dried over Na2SO4 and filtered. The filtrate was concentrated up to 14 (approximately 270 g) at reduced pressure.To the resulting solution, 80 ml of ethanol and 8.3 ml (100 mmol) of cone. HCl were added EPO and stirred at 24-26C for 3h. To the cooled mixture 600 ml of water was added and pH of the suspension was estimated to 5 by addition of 5 M NaOH. The phases were stirred for 15 min and separated. Water phase was reextracted with 150 ml of ethyl acetate. Collected organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure. 560 ml of ethyl acetate were added and the mixture was evaporated again. After that, 300 ml of ethyl acetate were added and the mixture was cooled to 20 0C and stirred for Ih, filtered off and washed with 20 ml of fresh ethyl acetate. The yield of the product (I) was 21 g (75 %).

The chemical industry reduces the impact on the environment during synthesis,80841-78-7,4-(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; KRKA; WO2007/17135; (2007); A2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Triphenyl methyl olmesartan, cas is 144690-92-6,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

A mixture of trityl olmesartan medoxomil in acetic acid and water (1:1, 400 mL) and sulfuric acid (12.2 gm) (1 mol equivalent) was stirred at 25C-30C for 45-60 minutes. Triphenylcarbinol was filtered and the filtrate was washed with acetic acid and water mixture (1:1, 50 rnL). Sodium carbonate solution (25% w/v, 100 mL) was charged to the filtrate and the product was extracted with dichloromethane (500 mL) followed by recovery of the solvent. The product was isolated, recrystallized using acetonitrile (300 mL), filtered, washed and dried under reduced pressure to obtain crude olmesartan medoxomil.Yield: 90% HPLC purity: 99.29 % OLM-acid: Not Detectable OLM- Eliminate: 0.07% Acetic acid content: Not Detectable

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of Triphenyl methyl olmesartan, 144690-92-6

Reference£º
Patent; RANBAXY LABORATORIES LIMITED; KAPOOR, Ashwini, Kumar; MEHTA, Hiten, Sharadchandra; NATH, Asok; PRASAD, Mohan; WO2010/134052; (2010); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Triphenyl methyl olmesartan, cas is 144690-92-6,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

Example 2: preparation of olmesartan medoxomil (I) as per the present invention: To a mixture of acetic acid ( 37.5 ml) and water (12.5 ml) was added trityl olmesartan medoxomil (III) (10 g) and heated at 40-45 C for 2 hours. Water (12.5 ml) was added and the reaction mixture was filtered to remove trityl alcohol. The filtrate was subjected to agitated thin film dryer, wherein the feed rate was of about 4 to 10 ml per minute, heating medium was jacketed hot water at 45-50 C and vacuum was 70-75 mm/Hg. Crude olmesartan medoxomil (I) was recovered form ATFD. HPLC purity: olmesartan medoxomil (I) (97.81 %); olmesartan acid impurity (II) (0.97%). To acetone (40 ml) crude olmesartan medoxomil (I) was added, the slurry was heated at 54-58 C for 30 minutes and then stirred for 1 -2 hours at 0-5 C, the solid was filtered. Wet solid was added to acetone (120 ml) and heated at 55-60C. The solution was filtered. From the filtrate about 95 ml of acetone was distilled out at atmospheric pressure. The concentrated mass was stirred at 25-30 C for 8-12 hours and then at 0-5 C for 1 -3 hours. The solid was filtered, washed with acetone and dried. Yield 5.3 g (76.81 %). HPLC purity: olmesartan medoxomil (I) (99.67 %); olmesartan acid impurity (II) (0.07%).

The chemical industry reduces the impact on the environment during synthesis,144690-92-6,Triphenyl methyl olmesartan,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; LUPIN LIMITED; FIRKE, Rajendra, Viswanath; SISODIA, Ujjwal,Komalsingh; BHANGALE, Chandrakant,Shriram; SHIVDAVKAR, Radhakrishna, Bhikaji; GODBOLE, Himanshu, Madhav; SINGH, Girij, Pal; WO2013/21312; (2013); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, cas is 80841-78-7,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

10L autoclave, 520g (0.75mol) Compound 5, DMF3kg, potassium carbonate and 215.3g (1.6mol), stirred at room temperature 1.5-2.5h added to the system after 63.0g (0.38mol) of potassium iodide was added dropwise while – Chloromethyl -5-methyl-1,3-dioxol-2-one 40.0g (0.94mol). Dropping was completed, the reaction at room temperature after 3-4h TLC or HPLC in control, raw reaction was complete. To the system was added ethyl acetate and 3L 3L water and 200g of sodium chloride, stirring separated and the aqueous layer was washed with 3X1L ethyl acetate, the combined organic layers, the organic layer was dried, filtered and the solvent was evaporated cooling is added 0-10 , methanol was added 1600g beating 30min, filtered, then the filter cake was slurried at room temperature in acetonitrile 1600g 30min, filtered to afford intermediate 6 about 553.8g,

The chemical industry reduces the impact on the environment during synthesis,80841-78-7,4-(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; Jiangsu Bang Pharmaceutical Co., Ltd.; Zhao, Guangrong; Huan, Shuang; Zhao, Huayang; Liu, Liping; Chen, Guoping; Tang, Jingyu; (19 pag.)CN105481842; (2016); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Triphenyl methyl olmesartan, cas is 144690-92-6,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

7.5 cm in diameterIn a 500 mL four-necked flask equipped with two stirring blades,40 g of trityl olmesartan medoxomil,180 ml of acetic acid,40 g (1.0 volume) of water was added,The mixture was stirred at 40 C. for 2 hours to carry out deprotection reaction (reaction conversion: 98.4%Olmesartan medoxomil purity: 98.95%,Olmesartan dimer: 0.047%).Then,The reaction solution was cooled to 20 C.,80 g of water was added,After stirring at 20 C. for 1 hour,The precipitated triphenylmethanol was removed by vacuum filtration,To the obtained filtrate, 240 ml of 10% sodium hydrogen carbonate was added,The liquidity of the aqueous layer was adjusted to pH 3.5,After adding 400 ml of ethyl acetate and vigorously stirring,The aqueous layer was separated,An organic layer containing olmesartan medoxomil was obtained (olmesartan medoxomil purity: 99.35%Dimer: 0.011%).200 ml of ethyl acetate was distilled off from the organic layer,After stirring at 20 to 30 C. for 1 hour,The precipitated solid was collected by filtration under reduced pressure as a wet body.The obtained wet body was dried at 40 C. for 14 hours,24 g of crystals of olmesartan medoxomil were obtained (yield: 86%, olmesartan medoxomil purity: 99.71%, dimer: 0.010%).

The chemical industry reduces the impact on the environment during synthesis,144690-92-6,Triphenyl methyl olmesartan,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Tokuyama Corporation; Mori, Hiroshi; Tanaka, Kenji; (12 pag.)JP6091339; (2017); B2;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, cas is 80841-78-7,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

Example 3; Preparation 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%

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, 80841-78-7

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

37830-90-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 4,5-Dimethyl-1,3-dioxol-2-one, cas is 37830-90-3,the Dioxole compound, it is a common compound, a new synthetic route is introduced below.

PREPARATION 1 4-Bromomethyl-5-methyl-2-oxo-1,3-dioxole To a stirred solution of 3.0 g of 4,5-dimethyl-2-oxo-1,3-dioxole in 100 ml of carbon tetrachloride was added 4.63 g of N-bromosuccinimide. The resulting solution was heated under reflux and irradiated for 15 minutes. The reaction mixture was cooled to 0¡ã-5¡ã C., filtered and evaporated to give the title product. The NMR spectrum (CDCl3) showed absorptions at 2.05 (5percent of starting material), 2.18 (3H, s), 4.30 (2H, s) and 4.35 (5percent of dibromo compound) ppm downfield from tetramethylsilane. The IR spectrum showed an absorption at 5.49 microns.

The chemical industry reduces the impact on the environment during synthesis,37830-90-3,4,5-Dimethyl-1,3-dioxol-2-one,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; Pfizer Inc.; US4434173; (1984); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

It is a common heterocyclic compound, the Dioxole compound, Triphenyl methyl olmesartan, cas is 144690-92-6 its synthesis route is as follows.

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, and the reaction was stirred until the amount of MTT was less than 2%. The mixture was evaporated to dryness. Ethyl acetate (EtOAc, 1 volume) was added to the residue and then evaporated again (twice). The resulting solid was dissolved in EtOAc (12 vol) and heated to reflux. The solution was cooled (2 C.) and stirred for 2 hrs. The product was filtered, washed (EtOAc, 1 vol), and dried on vacuum (45 C.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5

144690-92-6, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,144690-92-6 ,Triphenyl methyl olmesartan, other downstream synthetic routes, hurry up and to see

Reference£º
Patent; Hedvati, Lilach; Pilarsky, Gideon; Shenkar-Garcia, Natalia; US2006/148870; (2006); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Name is 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, as a common heterocyclic compound, it belongs to Dioxole compound, and cas is 80841-78-7, its synthesis route is as follows.

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%.

80841-78-7, In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles.,80841-78-7 ,4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, other downstream synthetic routes, hurry up and to see

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