Tag: M.W:100-200

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.,80841-78-7

Example 2; 36.0 g (50.3 mmol) ethyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-(4-[2-(trityltetrazol-5-yl)-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 0C and solution of 15.4 g (70.4 mmol) 4-chloromethyl-5-methyl-2-oxo-1,3-dioxolene in 39 ml of dimethylacetamide were slowly added. The mixture was slowly heated to 50C and stirred at this temperature for 2 h. After esterification was completed, the mixture was cooled to 10 C and poured into a mixture of 625 ml of ethyl acetate and 625 ml of 10 % NaCl, and stirred at 25 C for 15 min. The phases were separated and organic phase was washed 2x with 500 ml of 10 % NaCl, dried over Na2SO4 and filtered. The filtrate was concentrated up to ? (approximately 270 g) at reduced pressure. To the resulting solution, 80 ml of ethanol and 8.3 ml (100 mmol) of conc. HCl were added 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 C and stirred for 1h, filtered off and washed with 20 ml of fresh ethyl acetate. The yield of the product (I) was 21 g (75 %).

With the complex challenges of chemical substances, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

Reference£º
Patent; KRKA, tovarna zdravil, d.d., Novo mesto; EP1816131; (2007); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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

4725 g of dichloroethane was added to the DMDO that was stirred up.1012.5g N-chlorosuccinimideAnd 45g benzoyl peroxide,Reaction temperature 90¡ãC, reaction time 5.5h,The crude product obtained DMDO-Cl 382.5g, a yield of 85.00percent; Step 3: Distillation: The DMDO-Cl crude product at -0.1MPa vacuum,Distilled at 110¡ãC to produce 326g of DMDO-ClThe purity by gas chromatography was 99.06percent.

With the complex challenges of chemical substances, we look forward to future research findings about 4,5-Dimethyl-1,3-dioxol-2-one

Reference£º
Patent; Puyang Tianyuan Biological Technology Co., Ltd.; Zhao Junxia; Wen Jiaogang; Wang Lixia; Lv Xiaoyong; Fu Jingchao; Liu Renhuan; Chen Yongzhuang; Wang Lina; (6 pag.)CN107892681; (2018); A;,
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.,80841-78-7

(3) the C43 H39 N6 NaO3 AMST – 4 and DMF added in a reaction kettle, lowering the temperature to 0 C, adding potassium carbonate, maintain 0 C dropwise C5 H5 ClO3 AMST – 5 dissolved in DMF solution, after the completion of the dropping 85 C reaction 4 hours, monitoring the reaction is finished adding water, sodium chloride and ethyl acetate stirring extraction, liquid, separating the upper organic phase, a mixed solution of water and sodium chloride washing, separating the organic phase at upper layer for sodium sulfate drying, filtering, 60 C concentrated to the reagent, in acetonitrile for 30 C beating 1 hour, cooling to 25 C, filtering, cake isopropyl alcohol leaching, 75 C drying to constant weight to obtain the product C48 H44 N6 O6 AMST – 6; the C43 H39 N6 NaO3 AMST – 4, DMF, potassium carbonate, C5 H5 ClO3 AMST – 5, ethyl acetate, acetonitrile, water, sodium chloride and sodium sulfate the mass ratio of the 192:560: 62:1500: 1000:1500: 300:50;

With the complex challenges of chemical substances, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

Reference£º
Patent; Jiangxi Yong Tong Technology Co., Ltd.; Liu Zhongchun; (10 pag.)CN107311989; (2017); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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

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 is used more and more widely, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

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

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

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 is used more and more widely, we look forward to future research findings about 4,5-Dimethyl-1,3-dioxol-2-one

Reference£º
Patent; Metabasis Therapeutics, Inc.; US6054587; (2000); A;,
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,80841-78-7

1L glass reaction flask was added with 600ml of acetone, 114.8g of intermediate 1 was added with stirring, then 12.8g of sodium hydroxide was added, the temperature was raised to 50-60 C, and the reaction was incubated for 5 hours, and the reaction was monitored by HPLC. To 20-30 C, add 2.8g potassium iodide, 36.0g 4-chloromethyl-5-methyl-1,3-dioxol-2-one, and increase the temperature to 50-60 C after the addition After 1 hour of heat preservation reaction, the temperature was lowered to 20-30 C, filtered, and the filter cake was rinsed with 115 ml of acetone, and the filtrate was combined. The filtrate was concentrated under reduced pressure at 40-50 C until no obvious solvent flowed out, and 320 ml of acetonitrile was added to cool down. The mixture was decanted to 20-30 C for 1 hour, filtered, and the filter cake was rinsed with 320 ml of acetonitrile. The filter cake was blast dried at 40-50 C for 12 hours to obtain a white solid 110.0 g (intermediate 2). The rate was 85.8%, HPLC: 99.2%.

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

Reference£º
Patent; Jiashi (Hunan) Pharmaceutical Technology Co., Ltd.; Dai Yongzhi; Liu Hu; Zhu Laifa; Cai Jian; (8 pag.)CN108341804; (2018); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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

To a solution of the compound of Formula IV (5.0 g) in toluene (40 mL), dimethylacetamide (10 mL) is added, followed by addition of sodium hydroxide (1.2 g) and N,N-diisopropylamine (3.7 g) at 25-35C. The mixture is stirred at 40- 45C for 4 hours. 5-Methyl-2-oxo-(1 ,3-dioxolene-4-yl)methyl chloride (1.5 g) and tetrabutylammonium bromide (0.5 g) are added at 40-450C. The mixture is stirred at 60-70C for 8 hours. The mass is cooled to 25-35C, water (50 mL) is added, and the pH is adjusted to about 6-7 by adding 10% aqueous HCI. The layers are separated. The aqueous layer is extracted with toluene (25 mL). The organic layers are combined and washed with water (25 mL). The solvent is distilled under reduced pressure. Methanol (25 mL) is added to the residue. The mixture is cooled to 0-50C and stirred at that temperature for 45 minutes. The formed solid is filtered, washed with methanol (10 mL) and dried for 45 minutes under vacuum (yield 3.0 g).

80841-78-7 is used more and more widely, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

Reference£º
Patent; DR. REDDY’S LABORATORIES LTD.; DR. REDDY’S LABORATORIES, INC.; KOLLA, Naveen Kumar; MANNE, Nagaraju; NAREDLA, Anitha; SHINDE, Sachin Gulabrao; WO2011/14611; (2011); A2;,
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.,80841-78-7

To the flask was added 2000 g of acetone, 160 g of ethyl 4- (1-hydroxy-1-methylethyl) -2-propylimidazole-5-carboxylate (II), 150 g of K2CO3, 460 g of 4- [2- (Trityltetrazol-5-yl) phenyl] benzyl bromide (III), 20g KI, the temperature was raised to reflux, the reaction was incubated for 34-38 hours under stirring.Then add 102g KOH, reflux reaction 6 ~ 8h. Cool to 10 ~ 20 , add 170g DMDO-Cl, incubated for 30 ~ 60min.Heating to reflux, the reaction 22 to 26 hours.After the reaction was added 40g of diatomaceous earth, stirring for 30 to 60 minutes, suction filtration, 200g acetone rinse cake. To the filtrate was added 800g of drinking water and 200g of refined hydrochloric acid, the reaction at room temperature for 2 to 4 hours, filtered to remove by-product triphenylcarbinol. Dropping 10% K2CO3 aqueous solution, adjusting feedstock pH to 4, cooling to 10 ~ 20 , stirring crystallization 2h, filtration, the filter cake with a mixture of pre-cooled 45g acetone and 230g of drinking water washing and drying, to obtain Olmesartan Medoxomil 309 g, total yield 83.1% (relative to ethyl-4- (1-hydroxy-1-methylethyl) -2-propylimidazole-5- carboxylate (II)), purity: 99.27% of the main peak, 0.08% of the olmesartan acid, 0.14% of the triphenylmethanol, and 0.13% of the largest unidentified one.

With the complex challenges of chemical substances, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

Reference£º
Patent; Zhejiang Huahai Zhicheng Pharmaceutical Co., Ltd.; Zhejiang Huahai Pharmaceutical Co., Ltd.; Jin Congyang; Wang Jiquan; Zhang Wenling; Wang Peng; (10 pag.)CN107311990; (2017); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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

With the complex challenges of chemical substances, we look forward to future research findings about 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one

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

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.,37830-90-3

5. 0kg adding the compound of formula (IV) in a reaction vessel, 8. 0kg N- bromosuccinimide (NBS), 0. 30kg of azobisisobutyronitrile was added as the reaction solvent chloroform 100L, stirring was warmed to 38 ¡ã C, the reaction system to be stable, then slowly heated to reflux for 2-3 hours, the reaction was completed, cooled to room temperature, insolubles were removed by filtration, the filtrate was atmospheric recovery chloroform, 4 ¡ã C refrigerated overnight and filtered again after crystallization the insoluble matter was removed, and then distilled under reduced pressure collecting ll ¡ã C~120 ¡ã C / 5mmHg fractions, the compound of formula (V) 8. 66kg, yield (mole) 938percent, purity 95.1percent.;

With the complex challenges of chemical substances, we look forward to future research findings about 37830-90-3,belong Dioxole compound

Reference£º
Patent; Jumpcan Pharmaceutical Group/ji chuan(jiang su)Jumpcan Pharmaceutical Group co.ltd; cao, Longxiang; dong, Zibo; niu, ben; shao, Jianguo; (12 pag.)CN103113392; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem