Tag: M.W:100-200

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

Example 12: (5-Methyl-2-oxo-l,3-dioxol-4-yl)methyl 4-[(4-methoxyphenyl)amino]-6- (methylcarbamoy^quinoline-S-carboxylate. a) Preparation of the intermed 4-bromomethyl-5-methyl-2-oxo-l,3-dioxolene; To a solution of 4,5-dimethyl-l,3-dioxol-2-one (342 mg, 3.0 mmol) in carbon tetrachloride (10 mL) was added azobisisobutyronitrile (AIBN, 9.8 mg, 0.06 mmol) and iV-bromosuccinimide NBS (580 mg, 3.3 mmol). The reaction mixture was heated in the dark in a stem block at 78 C for 20 minutes. The mixture was cooled and evaporated almost into dryness. The mixture was filtered and the residue was evaporated to give a light yellow solid, which contained 20 percent starting material Yield: 450 mg (58percent). The mixture was used in the next step without further purifi- cation., 37830-90-3

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; CLANOTECH AB; MALM, Johan; RINGOM, Rune; CALDIROLA, Patrizia; WESTMAN, Jacob; WO2010/133669; (2010); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

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 infrared spectrum showed an absorption at 5.49 microns., 37830-90-3

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; Pfizer Inc.; US4448732; (1984); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

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.

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

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

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.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.

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; Metabasis Therapeutics, Inc.; US6054587; (2000); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

Step B, go to the reaction solution of compound (II) obtained in Step A with stirring,Add 6.27kg of anhydrous potassium carbonate powder and2.01kg iodine, replace the air with nitrogen, the nitrogen pressure in the kettle is ?0.01Mpa,The temperature was controlled at 50 ¡À 2 , and 13.80 kg of compound (IV) was added dropwise at a constant pressure.Add within 40 to 60 minutes. After the incubation reaction for 1.25 hours,Reduce the reaction mixture 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,Drying gave 55.03 kg of crude compound (I).Step C: Add 192.61 kg of ethyl acetate to the 500L refining kettle, start stirring,55.03 kg of the crude compound (I) obtained in step B is added, and the feeding port is closed,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.54.06kg compound (1) finished product,The HPLC content was 99.93%, and the residual content of the compound (III) was 0.05%.

The chemical industry reduces the impact on the environment during synthesis, 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; Shandong Xinhua Pharmaceutical Co., Ltd.; Zhu Lianbo; Wu Hui; Dou Guohua; (6 pag.)CN110590758; (2019); A;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

A solution containing about 46 g of compound 4 was taken, 3.5g sodium iodide was added, 280 mL N, N-dimethylformamide, 11.2g DMDO-Cl was slowly added dropwise, 30 Minute addition is completed. After dropping, Heated to 55 , Reaction for 7 hours, The reaction is completely over. filter, Remove insolubles, The filtrate was poured into 700mL of water, Extraction with ethyl acetate, The ethyl acetate layer was collected, dry, filter, The filtrate is concentrated. To the oily substance obtained after the concentration was added 200 mL of ethanol, Stirring, A white solid precipitation, Collect the solid, Washed with 50mL cyclohexane beating, 45.0 g of product was obtained, Two-step total yield of 80.6% The purity of the product was 98% by HPLC.

The chemical industry reduces the impact on the environment during synthesis, 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; Disha Pharmaceutical Group Co., Ltd.; Zhang Zhaoxing; Zhang Hongqiang; Qin Litai; Li Wei; Li Zongwen; Xia Haijian; (6 pag.)CN103012382; (2016); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

Step III: 4-Bromomethyl-5-methyl~l,3-dioxol~2-one; A mixture of 4,5-dimethyl-l,3-dioxol-2-one (1.5 g, 0.013158 mol), NBS (2.34 g, 0.013158 mol) and benzoyl peroxide (0.089 g, 0.0003684 mol) in CCl4 (20 mL) was stirred at 77¡ãC for 6 hrs (TLC monitoring: cyclohexane/AcOEt 6:4). The solution was treated with an aqueous solution OfNaHCO3 and extracted with CH2Cl2. The organic phase was dried over Na2SO4 and concentrated under reduced pressure to give 4-bromomethyl-5 -methyl- 1,3- dioxol-2-one (2.34 g). Yield: 92percent.1H-NMR (400 MHz, CDCl3, delta): 2.13 (s, 3H, CH3), 4.18 (s, 2H, CH2Br).

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; S.I.M.S. S.r.l. – SOCIETA ITALIANA MEDICINALI SCANDICCI; WO2008/12852; (2008); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

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, 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

4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.”80841-78-7

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%.

The chemical industry reduces the impact on the environment during synthesis, 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; INTERQUIM, S.A.; JOVE MARTI, Iban; MARQUILLAS OLONDRIZ, Francisco; WO2012/55994; (2012); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

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.37830-90-3, 4,5-Dimethyl-1,3-dioxol-2-one it is a common compound, a new synthetic route is introduced below.37830-90-3

A mixture of 4,5-dimethyl-1,3-dioxol-2-one (1.0 g, 8.8 mmol), benzoylperoxide (60 mg, 0.25 mmol) and N-bromosuccinimide (1.6 g, 9.0 mmol) in carbon tetrachloride (10 mL) was heated at reflux for 2 h. The solid was removed from the reaction mixture by filtration. The mother liquid was washed with sat. NaHCO3 and brine, dried over MgSO4 and concentrated. The crude product, 4-(bromomethyl)-5-methyl-1,3-dioxol-2-one, was obtained as a yellow oil (1.7 g) and was used without further purification in the next step.

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 4,5-Dimethyl-1,3-dioxol-2-one reaction routes.

Reference£º
Patent; Martinsson, Jessica; Faernegardh, Katarina; Joensson, Mattias; Ringom, Rune; US2015/25068; (2015); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem