Day: August 14, 2020

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.144690-92-6,Triphenyl methyl olmesartan,as a common compound, the synthetic route is as follows.

To 2000mL four-neck flask equipped with two stirring bladesof diameter 15 cm, tritylolmesartan medoxomil100 g, acetic acid450 ml, water 150mLwere added, & stirred for 2 hours at 40 C and deprotection reaction was carried out. Thereaction solution was then cooled to 20 C, stirred for 1 hour at 20 C, and precipitated triphenyl methanol wasremoved by filtrationunder reduced pressure, and to the resulting filtrate, 10% sodium bicarbonate 500ml, ethyl acetate1000ml were added and after vigorousstirrind, the aqueous layer was separated, to obtain an organic layercontaining olmesartanmedoxomil. ethylacetate 400ml was evaporated from the organic layer, and stirred for 1 hour at20 ~ 30 , and the precipitated solid was done filtration under reduced pressure and fractionated aswet product. The resulting wet product was dried for 14 hours at 40 , the crude olmesartan medoxomil wasobtained 60g(residual ethyl acetate content: 5420ppm, the residual amount of acetic acid:490ppm, purity: 99.37%). In 100mL three-necked flask equipped with two stirringblades of diameter 2.5 cm, crude olmesartan medoxomil 5g obtained in ProductionExample 1, acetone 15 ml, ethyl acetate 15 mL, water 3g were added and heatedto 60 C, to obtain a solution of olmesartan medoxomil (solution adjustingstep). then cooled to 30 C, and after adding seed crystals of olmesartanmedoxomil, it was stirred for 15 hours at 28 C (crystallization step: it wasconfirmed that there is no change in the amount of crystals even if it isretained for more time.) .

As the paragraph descriping shows that 144690-92-6 is playing an increasingly important role.

Reference£º
Patent; TOKUYAMA CORPORATION; MORI, HIROYUKI; TANAKA, KENJI; (13 pag.)JP2016/65007; (2016); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, Triphenyl methyl olmesartan is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

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%).

As the paragraph descriping shows that 144690-92-6 is playing an increasingly important role.

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.144690-92-6,Triphenyl methyl olmesartan,as a common compound, the synthetic 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 Triphenyl methyl olmesartan 19036162, aDioxole compound, is more and more widely used in various.

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.144690-92-6,Triphenyl methyl olmesartan,as a common compound, the synthetic route is as follows.

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 synthetic route of 144690-92-6 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; INTERQUIM, S.A.; JOVE MARTI, Iban; MARQUILLAS OLONDRIZ, Francisco; WO2012/55994; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The reaction flask was charged with 697.5 g of compound V obtained in the previous step,414 g of anhydrous potassium carbonate (3.00 mol)163.4 g of 4-chloromethyl-5-methyl-1,3-dioxol-2-one (Compound VI) (1.10 mol)And 2500 ml of acetonitrile were refluxed for 2 hours,After the reaction,filter,The filtrate was concentrated to dryness,The residue was stirred in 1500 ml of ethyl acetate and 500 ml of water for 15 minutes,Layered, organic layer and then washed with water,Dried over anhydrous sodium sulfate,filter,The filtrate was concentrated to dryness,To give the crude product of compound VII,Recrystallization from toluene and petroleum ether,To obtain pure product 683.2 grams; two-step yield:85.40% (calculated as compound II).

As the paragraph descriping shows that 80841-78-7 is playing an increasingly important role.

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

37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

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 synthetic route of 37830-90-3 has been constantly updated, and we look forward to future research findings.

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

144690-92-6, Triphenyl methyl olmesartan is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

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%.

144690-92-6 Triphenyl methyl olmesartan 19036162, aDioxole compound, is more and more widely used in various.

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

80841-78-7, 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 96.20 g of (III) were suspended in a mixture of 15.5 ml of tetrahydrofuran:dimethyl sulfoxide (2:3, v/v). The mixture was cooled to 17C in order to add 0.45 g (1.3 equivalents) of sodium hydroxide. The mixture was then heated to 60C. After two hours 1 .55 g (1 .1 equivalents) of potassium carbonate were added to the mixture. The mixture was heated to 70C and 1 .41 g of (IV) dissolved in 16.2 ml of tetrahydrofuran were added to the mixture over 1 .5 hours. The reaction was completed in one hour. The mixture was cooled to room temperature. The mixture was then washed three times with a 29% solution of sodium chloride in water. Finally, the organic solvent was distilled and 18.6 ml of ethyl acetate were added. Finally (V) was crystallised from ethyl acetate by cooling. The mixture was cooled to 0-5C, it was filtered, washed with ethyl acetate and heptane and the resulting solid was dried in a heat cabinet. 5.54 g of (V) were obtained (80% yield). The resulting solid was analysed by HPLC, showing a purity of more than 97%.

80841-78-7 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one 9855518, aDioxole compound, is more and more widely used in various.

Reference£º
Patent; INTERQUIM, S.A.; JOVE MARTI, Iban; MARQUILLAS OLONDRIZ, Francisco; WO2012/55994; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.37830-90-3,4,5-Dimethyl-1,3-dioxol-2-one,as a common compound, the synthetic route is as follows.

(1) Synthesis of 4-bromomethyl-5-methyl-1,3-dioxolen-2-one[the compound of formula (III) in which X is a bromine atom]: 3.42 g of 4,5-dimethyl-1,3-dioxolen-2-one (synthesised in accordance with Tetrahedron Letters, (1972), pages 1701-1704) was dissolved in 150 ml of carbon tetrachloride, and 5.34 g of N-bromosuccinimide and a catalytic amount of alpha,alpha’-azobisisobutyronitrile were added. The mixture was heated under reflux for 15 minutes. The reaction mixture was concentrated to half of its volume and the resulting insoluble matter was removed by filtration. Concentrating the filtrate gave a syrupy residue. The residue was distilled under reduced pressure to give a fraction boiling at 115¡ã to 120¡ã C./5 mm Hg which was 4.2 g (yield 73percent) of the captioned compound.

37830-90-3 4,5-Dimethyl-1,3-dioxol-2-one 142210, aDioxole compound, is more and more widely used in various.

Reference£º
Patent; Kanebo Ltd.; US4455310; (1984); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, Triphenyl methyl olmesartan is a Dioxole compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

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%.

144690-92-6 Triphenyl methyl olmesartan 19036162, aDioxole compound, is more and more widely used in various.

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