Tag: M.W:100-200

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 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.

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; Sawai Pharmaceutical Co., Ltd.; US5006548; (1991); 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.

(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.

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; Kanebo Ltd.; US4455310; (1984); 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.

REFERENCE EXAMPLE 2 Preparation of 4-chloromethyl-5-methyl-1,3-dioxolene-2-one (II) To a solution of 75 g of 4,5-dimethyl-1,3-dioxolene-2-one (IV) in 750 ml of methylene chloride was added 97.6 g of sulfuryl chloride dropwise at 40¡ã-42¡ã C. over 2 hours. The mixture was stirred for 40 minutes at the same temperature and evaporated in vacuo to remove the solvent. NMR spectrometry of the resulting oil revealed that the product was 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) containing a trace amount of unreacted 4,5-dimethyl-1,3-dioxolene-2-one (IV). This oil was heated at 90¡ã C. with stirring for 2 hours without isolating 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) and then distilled in vacuo. 75.4 g (corresponding to an overall yield from 4,5-dimethyl-1,3-dioxolene-2-one (IV) of 77percent) of 4-chloromethyl-5-methyl-1,3-dioxolene-2-one (II) having the physicochemical properties described in Reference Example 1 was obtained.

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; Kanebo, Ltd.; US4554358; (1985); 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

Example 7; Preparation of Trityl Olmesartan Medoxomil4-(1-Hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylic acid dehydrate (100 g) was suspended in acetone (1 L) & heated to reflux; the solution obtained was added to suspension of potassium carbonate (15 g), potassium iodide (6 g) & 4-chloromethyl-5-methyl-1,3-dioxol-2-one (35 g) in acetone (500 mL) at reflux temperature. Reaction mass was refluxed for 2-6 hrs. After competition of reaction, the reaction mass was filtered & the acetone was distilled from combined mother liquor. The residue obtained was dissolved in toluene (1 L) toluene layer was washed with brine (3¡Á250 mL). Toluene was removed under reduced pressure & residue thus obtained was recrystallized from methanol to give trityl OlmesartanMedoxomil (100 g).HPLC purity=99.5%

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; Ramanjaneyulu, Gorantla Seeta; Mohan, Bandari; Ray, Purna Chandra; Sethi, Madhuresh Kumar; Rawat, Vijendra Singh; Krishna, Yerramalla Raja; Lakshminarayana, Vemula; Srinivas, Mamidi; US2009/281327; (2009); 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

REFERENCE EXAMPLE 2 Preparation of 4-chloromethyl-5-methyl-1,3-dioxolene-2-one (II) To a solution of 75 g of 4,5-dimethyl-1,3-dioxolene-2-one (IV) in 750 ml of methylene chloride was added 97.6 g of sulfuryl chloride dropwise at 40¡ã-42¡ã C. over 2 hours. The mixture was stirred for 40 minutes at the same temperature and evaporated in vacuo to remove the solvent. NMR spectrometry of the resulting oil revealed that the product was 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) containing a trace amount of unreacted 4,5-dimethyl-1,3-dioxolene-2-one (IV). This oil was heated at 90¡ã C. with stirring for 2 hours without isolating 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) and then distilled in vacuo. 75.4 g (corresponding to an overall yield from 4,5-dimethyl-1,3-dioxolene-2-one (IV) of 77percent) of 4-chloromethyl-5-methyl-1,3-dioxolene-2-one (II) having the physicochemical properties described in Reference Example 1 was obtained.

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; Kanebo, Ltd.; US4554358; (1985); A;,
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,37830-90-3

EXAMPLE 1 Preparation of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) To a solution of 50 g of 4,5-dimethyl-1,3-dioxolene-2-one (IV)(Synthesised by the method described in Tetrahedron Letters, 1701-1704 (1972)) in 350 ml of methylene chloride was added 65 g of sulfuryl chloride dropwise over 1 hour at 40¡ã-42¡ã C. The mixture was stirred for one hour at the same temperature and then evaporated in vacuo to remove the solvent. The resulting residue was distilled in vacuo to obtain 42.1 g (65percent of theory) of 4-chloro-4-methyl-5-methylene-1,3-dioxolane-2-one (III) as a colorless oil. B.p. 45¡ã-48¡ã C./2 mmHg. IR(CHCl3)nu(cm-1): 1820, near 1695 etc. NMR(CDCl3, delta(ppm)): 2.19(3H, s, CH3), STR5

As the paragraph descriping shows that 37830-90-3 is playing an increasingly important role.

Reference£º
Patent; Kanebo, Ltd.; US4554358; (1985); A;,
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.

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.

#REF!

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

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.

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 4Preparation of trityl 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 potassium hydroxide (25 gms). To this was charged 4-[2-(trityltetrazol-5-yl)phenyl]benzyl bromide (135 gms) at 45-500C. The contents were stirred for 5 hours at 45-500C. Diisopropylethyl amine (100 ml) was charged to the reaction mass at 40-45C. To this was slowly added a solution of 5-methyl-2-oxo- 1 ,3-dioxane-4-yl) methyl chloride (80 gms) diluted with dimethyl acetamide (160 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 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 quenched with purified water(200 ml)at 25-30C over a period of 3-4 hours. The contents were stirred at 25-300C for 30 minutes. Crude trityl olmesartan medoxomil was isolated by filtration, slurried in water (500 ml), centrifuged and dried under reduced pressure at 45-50C.

#REF!

Reference£º
Patent; CIPLA LIMITED; CURTIS, Philip, Anthony; WO2008/43996; (2008); A2;,
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

(1) 2.08 g of 4,5-dimethyl-1,3-dioxol-2-one was dissolved in 24 mL of benzene, to which 3.25 g of N-bromosuccinimide and 86 mg of 2,2′-azobis(isobutyronitrile) were added at room temperature, and this mixture was stirred for 30 minutes while heating it under reflux. The reaction mixture was cooled to room temperature, and consequently, a solution of 4-bromomethyl-5-methyl-1,3-dioxol-2-one in benzene was obtained.(2) 3.00 g of methyl 3-(5-[4-(cyclopentyloxy)-2-hydroxybenzoyl]-2-{[3-(methoxymethoxy)-1,2-benzisoxazol-6-yl]methoxy}phenyl) propanoate was dissolved in 15 mL of methanol and 15 mL of tetrahydrofuran, to which a solution of 1.08 g of potassium hydroxide in 4.5 mL of water was added, and this mixture was stirred for one hour at room temperature, and then the solvent was distilled out under reduced pressure. The resultant residue was dissolved in 40 mL of N,N-dimethylformamide, to which 3.60 g of potassium carbonate was added. Then, the benzene solution prepared in (1) was added thereto, and was stirred for one hour at room temperature. The reaction mixture was poured into a mixture of ethyl acetate and water, and adjusted to pH 7 with 6M hydrochloric acid, and then the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous sodium sulfate, and the solvent was distilled out under reduced pressure. The resultant residue was purified by silica gel column chromatography [eluent; toluene:ethyl acetate=5:1] to yield 1.58 g of (5-methyl-2-oxo-1,3-dioxol-4-yl)methyl 3-(5-[4-(cyclopentyloxy)-2-hydroxybenzoyl]-2-{[3-(methoxymethoxy)-1,2-benzisoxazol-6-yl]methoxy}phenyl) propanoate as yellow oil. NMR(400MHz,CDCl3) delta value: 1.5-2.0(8H,m), 2.16(3H,s), 2.75(2H,t,J=7.6Hz), 3.10(2H,t,J=7.6Hz), 3.65(3H,s), 4.5-5.0(3H,m), 5.33(2H,s), 5.57(2H,s), 6.37(1H,dd,J=8.8,2.4Hz), 6.47(1H,d,J=2.4Hz), 6.95(1H,d,J=8.4Hz), 7.35(1H,dd,J=8.4,1.2Hz), 7.4-7.6(4H,m), 7.72(1H,d,J=8.0Hz), 12.67(1H,s).

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; TOYAMA CHEMICAL CO., LTD.; Hirono, Shuichi; Shiozawa, Shunichi; EP1445249; (2004); 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

Example 1The feeding substance than the molar amount of the: DMDO: sulfonyl chloride to 1 : 1.3. The organic solvent is dichloromethane, the quality of the organic solvent with DMDO volume ratio is 1:7. Solid free radical scavenging agent is methyl hydroquinone, DMDO the quality of the amount of 1percent.To is provided with a magnetic stirring, constant pressure dropping funnel, reflux condensation tube, thermometer and is provided with a tail gas absorption device 500 ml flask to three in 350 ml dichloromethane, 50gDMDO, under stirring backflow state, slowly dropping 77g sulfonyl chloride, dropping time is approximately 2.5h, heat preservation after dropping 2h, rotary evaporation to remove the solvent. Furthermore, added to the bottoms of 0.5g methyl hydroquinone, for 90 ¡ãC conditions, stirring rearrangement 5h, obtaining a reaction crude. Analysis of the purity of crude 92.33percent, the crude in 2mmHg the vacuum degree of the vacuum distillation, to obtain the target product 52.8g, to yield 81.1percent, purity of 97.87percent.

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; Six Anke Rui Da New Materials Co.,Ltd.; Bao, Yuanzhi; Weng, Shibing; Zhao, Zhongyao; (6 pag.)CN105348249; (2016); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem