Day: September 1, 2020

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

[01658] A solution of 4,5-dimethyl-2-oxo-1,3-dioxolene (1 mmole) and selenium dioxide (2.5 mmole) 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: RPf=0.5, 5percent MeOH-dichloromethane. [01659] A solution of 5-methyl-4-hydroxymethyl-2-oxo-1,3-dioxolene (1 mmole) in DMF was treated with tert-butyldimethylsilane (1.2 mmole) and imidazole (2.2 mmole) at 25 C. for 24 h. Extraction and chromatography gave 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-oxo-1,3-dioxolene. [01660] A solution of 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-oxo-1,3-dioxolene (1 mmole) and Lawesson’s reagent (1.2 mmole) in toluene was heated to 120 C. for 12 h. Extraction and chromatography gave 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-thio-1,3-dioxolene. [01661] A solution of 5-methyl-4-tert-butyldimethylsilyloxymethyl-2-thio-1,3-dioxolene in methanolic hydrogen chloride was stirred at 0 C. for 1 h and 25 C. for 12 h. Extraction and chromatography gave 5-methyl-4-hydroxymethyl-2-thio-1,3-dioxolene.

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

Reference£º
Patent; Metabasis Therapeutics, Inc.; US6756360; (2004); B1;,
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

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%.

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

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

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

Trityl olmesartan medoxomil (8 g, 10 mmol) is added to a mixture of acetone (35 ml) and water (10 ml). To the resulting suspension 37 % aqueous hydrochloric acid (2.5 ml, 30 mmol) is added. The mixture is then stirred at room temperature for 4 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 hydrochloride Form A (98.3 % area)

With the rapid development of chemical substances, we look forward to future research findings about Triphenyl methyl olmesartan

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

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

A mixture of trityl olmesartan medoxomil in acetic acid and water (1:1, 400 mL) and sulfuric acid (12.2 gm) (1 mol equivalent) was stirred at 25C-30C for 45-60 minutes. Triphenylcarbinol was filtered and the filtrate was washed with acetic acid and water mixture (1:1, 50 rnL). Sodium carbonate solution (25% w/v, 100 mL) was charged to the filtrate and the product was extracted with dichloromethane (500 mL) followed by recovery of the solvent. The product was isolated, recrystallized using acetonitrile (300 mL), filtered, washed and dried under reduced pressure to obtain crude olmesartan medoxomil.Yield: 90% HPLC purity: 99.29 % OLM-acid: Not Detectable OLM- Eliminate: 0.07% Acetic acid content: Not Detectable

With the rapid development of chemical substances, we look forward to future research findings about Triphenyl methyl olmesartan

Reference£º
Patent; RANBAXY LABORATORIES LIMITED; KAPOOR, Ashwini, Kumar; MEHTA, Hiten, Sharadchandra; NATH, Asok; PRASAD, Mohan; WO2010/134052; (2010); A1;,
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

PREPARATION 18 4-Carbo-(5-methyl-2-oxo-1,3-dioxol-4-ylmethoxy)methylpiperazine hydrochloric acid salt Combine 4,5-dimethyl-1,3-dioxol-2-one (3.42 g, 30 mmol), N-bromosuccinimide (5.34 g, 30 mmol) and AIBN (500 mg, 3 mmol) in anhydrous carbon tetrachloride (100 mL). Heat at reflux. After 2 hours, cool and filter. Concentrate the filtrate to give 4-bromomethyl-5-methyl-1,3-dioxol-2-one (6.5 g, crude) as an oil, which can be used for the next step without further purification.

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

Reference£º
Patent; Hoechst Marion Roussel, Inc.; US5977139; (1999); 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

To a stirred solution of 4, 5-dimethyl-l, 3-dioxol-2-one (4.5 g, 39.4 mmol) in benzene (150 mL), were added NBS (15.44 g, 87 mmol) and AIBN (0.648 g, 3.94 mmol). The reaction mixture was stirred at 1 10 C for 2 h under nitrogen atmosphere and subsequently concentrated in vacuo. The residue was dissolved in ethyl acetate (200 mL). The solution was washed with water (2* 150 mL) and brine (100 mL), dried over anhydrous sodium sulphate and concentrated in vacuo to get the crude product as a light brownish oil, which was purified by CombiFlash chromatography (60-120 silica gel; 5- 55% ethyl acetate in pet. ether as eluent) to afford 4,5 -bis (bromomethyl)-l,3-dioxol-2- one (7 g, 66%) as a light yellowish oil. NMR (400 MHz, Chloroform-7) d ppm 4.22 (s, 4H).

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

Reference£º
Patent; BRISTOL-MYERS SQUIBB COMPANY; BALOG, James Aaron; SEITZ, Steven P.; WILLIAMS, David K.; ANDAPPAN MURUGAIAH SUBBAIAH, Murugaiah; (191 pag.)WO2019/136112; (2019); A1;,
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

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).

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

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

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.,144690-92-6

A solution of MTT in 10 volumes of acetic acid (75%) was heated for 1.5 hrs at 60 C. until a pH of 2.21-2.23 was achieved, 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.).

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

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.80841-78-7,4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one,as a common compound, the synthetic route is as follows.,80841-78-7

Example 1-5 (0330) (0331) A mixture of BIC (0.6 g, 0.83 mmol), potassium iodide (0.069 g, 0.41 mmol), OXC (0.245 g, 1.65 mmol) and methyl ethyl ketone (9.0 mL, 15 vol) was stirred at 50 C. for 20 hr. The reaction mixture was filtered, the filtrate was concentrated under reduced pressure, and the obtained concentrated residue was purified by silica gel column chromatography (20-22% ethyl acetate/hexane) to give TOLM (650 mg, yield 84.4%). (0332) Mass: 801 [M+H]+, 824 [M+Na]+.

The synthetic route of 80841-78-7 has been constantly updated, and we look forward to future research findings.

Reference£º
Patent; API CORPORATION; Seki, Masahiko; US2015/239854; (2015); A1;,
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,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)

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

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