Dioxole related

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

37830-90-3, To a solution of 4,5-dimethyl-1,3-dioxolene-2-one (TCI, 10 g, 88 mmol) and N- bromosuccinimide (Fluka, 15.69 g, 88 mmol) in carbon tetrachloride (250 mL) was added benzoyl peroxide (Acros, 500 mg, 2.1 mmol). The reaction mixture was then refluxed for 2.5 h after which time the volatiles were evaporated under vacuum. The resulting residue was triturated with some carbon tetrachloride, filtered and the solid cake was washed with carbon tetrachloride. The filtrate volatiles were removed under vacuum and the yellow oily residue was distilled under vacuum (2-5 torr) to give 4-bromomethyl-5-methyl-1,3-dioxolene-2-one 903 (8.35 g, b.p. 94-98 ¡ãC, 49percent) as a pale yellow oil. 1H NMR (CDCI3) 8 4.21 (s, 2H), 2.17 (s, 3H).

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; RIGEL PHARMACEUTICALS, INC.; WO2005/97760; (2005); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, 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.”144690-92-6

Trityl olmesartan medoxomil (8 g, 10 mmol) is dissolved in THF (50 ml) and 48 % aqueous hydrobromic acid (3.5 ml, 30 mmol) is added. The mixture is stirred for 1 hour at room temperature and then 1 hour at 0 C. The precipitate is filtered, washed with cold THF (20 ml) and dried overnight in vacuum at room temperature to give 5.7 g of olmesartan medoxomil hydrobromide Form B (98.6 % area)

With the synthetic route has been constantly updated, we look forward to future research findings about Triphenyl methyl olmesartan,belong Dioxole compound

Reference£º
Patent; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

144690-92-6, 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.”144690-92-6

Example 1 – formation of olmesartan medoxomil hydrobromide Form A Trityl olmesartan medoxomil (8 g, 10 mmol) is added to a mixture of acetone (35 ml) and water (10 ml). To the resulting suspension 48 % aqueous hydrobromic acid (3.5 ml, 30 mmol) is added. The mixture is then stirred at room temperature for 2 h. Water (130 ml) is added and the mixture is stirred for additional 30 minutes. The precipitated triphenylmethanol is filtered off. The filtrate is concentrated in vacuum at 40 C to 100 ml, and then stirred vigorously for 1 h at room temperature and then additional 30 minutes at 0 C. The precipitate is filtered to give 4.7 g of olmesartan medoxomil hydrobromide Form A (97.6 % area); Example 9 – formation of olmesartan medoxomil Trityl olmesartan medoxomil (18 g, 22.5 mmol) (95.5 % area) is added to a mixture of acetone (68 ml) and water (22 ml). To the resulting suspension 48 % aqueous hydrobromic acid (8.5 ml, 72 mmol) is added. The mixture is then stirred at room temperature for 2 h. Water (180 ml) is added and the mixture is stirred for additional 15 minutes. The precipitated triphenylmethanol is filtered off. The filtrate is concentrated in vacuo at 40 C to 200 ml and then stirred vigorously for 20 minutes at room temperature and then additional 40 minutes at 0 C. The precipitate is filtered and dried overnight in vacuum at 25 C to give 12.9 g of olmesartan medoxomil hydrobromide Form A. This was added to THF (150 ml) and the mixture is stirred vigorously for 30 minutes at room temperature and 1 hour at 0 C. The precipitate is filtered and washed with 25 ml of cold THF to give olmesartan medoxomil hydrobromide Form B, which is then dissolved in a mixture of water (100 ml) and acetone (50 ml). To a clear solution saturated aqueous NaHCO3 is added to raise pH to 5.6. The mixture is stirred for 1 hour at room temperature and 2 hours at 0 C. The precipitate is filtered, washed with water and then recrystallised from acetonitrile (87 ml) to give 8.3 g of olmesartan medoxomil (99.74 % area), 144690-92-6

With the rapid development of chemical substances, we look forward to future research findings about 144690-92-6

Reference£º
Patent; LEK Pharmaceuticals d.d.; EP2022790; (2009); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

80841-78-7, 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

(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

144690-92-6, 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.”144690-92-6

Example 236.0 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 0 C. 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 50 C. 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 2¡Á 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 24-26 C. for 3 h. 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 1 h, 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, Triphenyl methyl olmesartan, , I believe this compound will play a more active role in future production and life.

Reference£º
Patent; KRKA; US2009/131680; (2009); 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

Example 236.0 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 0 C. 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 50 C. 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 2¡Á 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 24-26 C. for 3 h. 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 1 h, 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, 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; US2009/131680; (2009); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

Name is Triphenyl methyl olmesartan, as a common heterocyclic compound, it belongs to Dioxole compound, and cas is 144690-92-6, its synthesis route is as follows.

Example 5; Olmesartan medoxomil (V); Water (10 g) was added to a solution of the starting substance (III; 20 g) in acetonitrile (50 ml), and the mixture was heated to a mild boil for 14 h. Acetonitrile was evaporated, and, after dissolving in acetone (150 ml), the mixture was filtered through alumina and concentrated. After crystallization from the mixture tetrahydrofuran / ethyl acetate H g (78 %) of the product with an HPLC purity of 97.0 % was obtained. Recrystallization from methanol and water gave 1O g of the product with an HPLC purity of 99.3 %; m.p. 175- 177 0C.; Example 6; Olmesartan medoxomil (V); Water (10 g) was added to a solution of the starting substance (III; 10 g) in acetonitrile (50 ml), and the mixture was heated to a mild boil for 14 h. Acetonitrile was evaporated, and, after dissolving in acetone (150 ml), the mixture was filtered through silica gel and concentrated. After crystallization from acetonitrile, 4 g (57 %) of the product was obtained. After recrystallization from the mixture methyl tert-butyl ether / ethyl acetate, 3.4 g of the product with an HPLC purity of 99.4 % was obtained; m.p. 175-177 C.

144690-92-6, 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.,144690-92-6 ,Triphenyl methyl olmesartan, other downstream synthetic routes, hurry up and to see

Reference£º
Patent; ZENTIVA, A.S.; WO2007/48361; (2007); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem

As a common heterocyclic compound, it belongs to Dioxole compound, name is Triphenyl methyl olmesartan, and cas is 144690-92-6, its synthesis route is as follows.

(4) the C48 H44 N6 O6 AMST – 6, acetone, water, sulfuric acid added to the reactor, the temperature rising to 30 C reaction 2.5 hours, adding water, 30 C continue to reaction 1.5 hours or more, when the raw material to achwhich isve the requirement of lowering the temperature to 5 C stirring 1 or more hours, filtering the triphenyl methanol, the filter cake is washed with water; mother liquor up to 50 C, add sodium bicarbonate, stirring 1 hour, filtration products, the filter cake is washed with water, 50 C decompression drying 12 hours or more to constant weight, to obtain omay sha tanzhi thick; said C48 H44 N6 O6 AMST – 6, acetone, water, sulfuric acid and sodium bicarbonate and the mass ratio of 700:1400:: 2101.4: 194.7: 373.5; (5) the crude product of olmesartan medoxomil and acetone is added to the reaction in the bottle, heat to reflux to totally dissolve, filter press, distilling off acetone, lowering the temperature to -10 C crystallization, filtration, acetone washing, 50 C drying productC29 H30 N6 O6 Olmesartan medoxomil, the crude with olmesartan medoxomil mass ratio of olmesartan medoxomil 448.4: 6500;

144690-92-6, 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.,144690-92-6 ,Triphenyl methyl olmesartan, other downstream synthetic routes, hurry up and to see

Reference£º
Patent; Jiangxi Yong Tong Technology Co., Ltd.; Liu Zhongchun; (10 pag.)CN107311989; (2017); 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) 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).

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; TOYAMA CHEMICAL CO., LTD.; Hirono, Shuichi; Shiozawa, Shunichi; EP1445249; (2004); A1;,
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.

Add 50.0 g of 4,5-dimethyl-1,3-dioxol-2-one to a 1 L four-necked flask.530 g of dichloromethane, stirred and dissolved, and heated to reflux, when the internal temperature is not lower than 40 ¡ã C,A mixture of 65 g (1.1 equivalents) of sulfonyl chloride and 132 g of dichloromethane was added dropwise.The internal temperature of the control is not lower than 40 ¡ãC, and the mixture is kept warm for 2 hours after the dropwise addition.The temperature was then raised to 85 ¡ã C while distilling off the dichloromethane. When it reaches 85 ¡ã C, it is rearranged for 2 to 3 hours.At room temperature, crude DMDO-Cl was obtained with a GC purity of 85percent to 90percent.Add 30 ml of isopropanol to the above crude product, stir and cool to -10 ¡ã C ~ -5 ¡ã C,Crystallization 0 ~ 1h, suction filtration, rinse with isopropanol down to -5 ¡ã C,Obtained white crystals 53.3g (yield 81.9percent, GC purity 99.3percent)

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; Zhejiang Huahai Pharmaceutical Co., Ltd.; Wang Jiquan; Li Guoxiang; Xiong Xueqiang; (6 pag.)CN103864748; (2019); B;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem