Day: September 18, 2020

As a common heterocyclic compound, it belongs to Dioxole compound, name is 4,5-Dimethyl-1,3-dioxol-2-one, and cas is 37830-90-3, its synthesis route is as follows.

Example 26 Preparation of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene A mixture of 4,5-dimethyl-2-oxo-1,3-dioxolene (1 mmol) and selenium dioxide (2.5 mmol) in dioxane was heated at reflux for 1 h. Evaporation, extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene as a yellow oil. TLC: Rf=0.5, 5percent MeOH-dichloromethane.

37830-90-3, 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.,37830-90-3 ,4,5-Dimethyl-1,3-dioxol-2-one, other downstream synthetic routes, hurry up and to see

Reference£º
Patent; Metabasis Therapeutics, Inc.; US6054587; (2000); A;,
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.

Example 17 Preparation of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene A solution of 4,5-dimethyl-2-oxo-1,3-dioxolene (1 mmol) and selenium dioxide (2.5 mmol) in dioxane was heated at reflux for 1 h. Evaporation, extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene as a yellow oil. TLC: Rf=0.5, 5percent MeOH-dichloromethane.

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 4,5-Dimethyl-1,3-dioxol-2-one, 37830-90-3

Reference£º
Patent; Metabasis Therapeutics, Inc.; US6284748; (2001); B1;,
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 1323.88 g of (V) were suspended in 92 ml of acetonitrile. The mixture was cooled to 5C in order to add 24.6 ml of 6N HCI. The mixture was stirred for 2 hours at 5C. 150 ml of toluene were added. The pH was adjusted to 5.7 with potassium bicarbonate. The mixture was filtered in order to eliminate part of the salts generated. The solid was washed with 30 ml of acetonitrile. The phases were separated. The acetonitrile present in the organic phase was distilled. The mixture was cooled and filtered. The solid was washed with toluene and water. (VI) was dried in a heat cabinet. 16.66 g of (VI) were obtained (85% yield).

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; INTERQUIM, S.A.; JOVE MARTI, Iban; MARQUILLAS OLONDRIZ, Francisco; WO2012/55994; (2012); 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.

Trityl olmesartan medoxomil (260 gm) as obtained in example 1 was dissolved in toluene (2600 ml) and then added concentrated hydrochloric acid (156 ml) for 1 hour minutes at room temperature. The reaction mass was maintained for 1 hour 30 minutes at room temperature and then added water (1000 ml). The reaction mass was stirred for 45 minutes at room temperature and the layers were separated. To the aqueous layer was added ethyl acetate (5000 ml) at room temperature. The reaction mass was cooled to 15 to 20 C. and pH of the reaction mass was adjusted to 4.5 to 5.5 with sodium carbonate (20%, 560 ml). The reaction mass was stirred for 20 minutes at 20 C. and the layers were separated. The organic layer was dried over sodium sulfate and ethyl acetate was distilled off completely under vacuum at below 45 C. to obtain a residual mass. To the residual mass was added ethyl acetate (400 ml) at 40 C. and then heated to 75 to 80 C. The contents were maintained for 30 minutes at 75 to 80 C. The reaction mass was cooled to room temperature and stirred for 1 hour. The reaction mass was further cooled to 10 to 15 C. and stirred for 1 hour 30 minutes, filtered. The solid obtained was dried at 40 to 45 C. for 4 hours to obtain 150 gm of olmesartan medoxomil. Olmesartan medoxomil: 98.6%; Olmesartan acid impurity: 0.32%; Trityl olmesartan medoxomil impurity: 0.35% Methyl olmesartan medoxomil impurity: 0.35%.

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; HETERO RESEARCH FOUNDATION; Parthasaradhi Reddy, Bandi; Rathnakar Reddy, Kura; Muralidhara Reddy, Dasari; Raji Reddy, Rapolu; Ramakrishna Reddy, Matta; Vamsi Krishna, Bandi; US2013/190506; (2013); 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.

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