Month: August 2020

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

78(b) (5-Methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(tetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate 75 ml of water were added to a suspension of 29.3 g of (5-methyl-2-oxo-1,3-dioxolen-4-yl)methyl 4-(1-hydroxy-1-methylethyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]phenyl}methylimidazole-5-carboxylate [prepared as described in step (a) above] in 225 ml of acetic acid, and the resulting mixture was stirred at 60 C. for 1.5 hours. At the end of this time, 75 ml of water were added to the mixture, which was then cooled. Precipitated trityl alcohol was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure. Toluene was added to the residue, and the mixture was again concentrated by evaporation under reduced pressure, to remove the remaining water and acetic acid. The residue was crystallized in ethyl acetate, to give 16.6 g of the title compound as crystals, melting at 177-180 C. (with decomposition). The Nuclear Magnetic Resonance Spectrum of this compound was identical with that of the compound obtained as described in Example 61(b).

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

Reference£º
Patent; Sankyo Company, Limited; US5616599; (1997); 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

A solution of MTT in an organic solvent and water (20%) was heated for 4-8 hrs at reflux. When the solvents were either acetonitrile (ACN), isopropyl alcohol (IPA) or t-butanol (t-BuOH), 1 volume of water was added, 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.). Table 1 shows the process details with different organic solvents: TABLE 1 Total solvent Time Solvent(s) Volume Temperature ( C.) (hrs) pH ACN:H2O 5:1 + 1 85 7 4.89-4.3 IPA:H2O 5:1 + 1 85 7 4.62-4.25t-BuOH:H2O 5:1 + 1 85 7 4.78-4.28n-propanol:H2O 5:1 reflux 2.5 4.3n-BuOH:H2O 5:1 110 2.5 4.412-BuOH:H2O 5:1 100 3 4.5iso-penthanol:H2O 5:1 100 3 5DMA:H2O 5:1 100 4 4.5DMF:H2O 5:1 100 4 4.5

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

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.37830-90-3,4,5-Dimethyl-1,3-dioxol-2-one,as a common compound, the synthetic 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.

The synthetic route of 37830-90-3 has been constantly updated, and we look forward to future research findings.

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

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

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

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

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

Trityl olmesartan medoxomil (250 g, 310 mmol) (97.3 % area) is dissolved in THF (1560 ml) and 48 % aqueous hydrobromic acid (70.6 ml, 625 mmol) is added slowly. The mixture is stirred for at 25 C. After 1 hour the precipitate forms. The mixture is stirred for 1 additional hour at 25 C, then cooled to -5 C and stirred for 1.5 hours at -5 C. The precipitate is filtered. 940 ml of THF is added to the precipitate and the mixture is stirred for 1 h at 25 C and then 1 hour at -5 C. Then precipitate is filtered off and washed with cold THF (150 ml). It is then dissolved in a mixture of water (875 ml) and acetone (440 ml). To a clear solution 5 % aqueous solution of NaHCO3 is added to raise pH to 5.15. The mixture is stirred for 1 hour at room temperature and 1 hour at 0 C. The precipitate is filtered, washed with water and then recrystallized from a mixture of acetonitrile (280 ml) and water (70 ml) to give 124.5 g of olmesartan medoxomil (99.68 % 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

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

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 %).

144690-92-6 Triphenyl methyl olmesartan 19036162, aDioxole compound, is more and more widely used in various.

Reference£º
Patent; KRKA, tovarna zdravil, d.d., Novo mesto; EP1816131; (2007); 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

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 4-(Chloromethyl)-5-methyl-1,3-dioxol-2-one 9855518, aDioxole compound, is more and more widely used in various.

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.37830-90-3,4,5-Dimethyl-1,3-dioxol-2-one,as a common compound, the synthetic route is as follows.,37830-90-3

Compound 20 was prepared following the steps disclosed in the literature (Sakamoto er a/., Chem. Pharm. Bull, 1984, 32, 2241).

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

Reference£º
Patent; ANCHEN LABORATORIES, INC; WO2009/118580; (2009); A2;,
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

Example 1-6 (0333) (0334) A mixture of TOLM (0.6 g, 0.75 mmol), sulfuric acid (0.08 g, 0.82 mmol) and 1:1 water-containing acetic acid (2.6 mL, 4.3 vol) was stirred at 25 C. for 1 hr. The reaction mixture was filtered, and the obtained solid was washed with 1:1 water-containing acetic acid (6.0 mL, 10 vol). The filtrates were combined and adjusted to pH 4-5 by adding 25% aqueous sodium carbonate solution. The mixture was partitioned by adding methylene chloride (6.0 mL, 10 vol). The aqueous layer was extracted with methylene chloride (3¡Á5 mL). The organic layer was washed with water (2¡Á5 mL) and saturated brine (5 mL), and concentrated under reduced pressure. The concentrated residue was purified by silica gel column chromatography (5-6% methanol/methylene chloride) and recrystallized from acetonitrile to give OLM (0.45 g, yield 100%). (0335) melting point: 174.5 C.-175.2 C.; (0336) IR (KBr): numax=2969, 1831, 1706, 1475, 1226, 1134, 760 cm-1; (0337) 1H NMR (DMSO-d6): delta=7.70-7.63 (m, 2H), 7.59-7.52 (m, 2H). (0338) 7.04 (d, J=8 Hz, 2H), 6.85 (d, J=8.4 Hz, 2H), 5.42 (s, 2H), 5.21 (s, 1H), 5.05 (s, 2H), 2.60 (t, J=7.6 Hz, 2H), 2.07 (s, 3H), 1.60-1.55 (m, 2H), 1.47 (s, 6H), 0.87 (t, J=7.2 Hz, 3H); (0339) Mass: 559 [M+H]+.

The synthetic route of 144690-92-6 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

To 12.0g (15 mmol) of tritylolmesartan medoxomil prepared according to examples 1 or 2 69 ml of ethyl acetate was added and after that 12 ml of methanol and 2.67 ml (32 mmol) of conc. HCl were added. The mixture was stirred at room temperature for 2h and then the mixture was cooled to below 2C. To the cooled mixture 71 ml of 1% NH3 was slowly added to adjust pH to 4.93. The phases were separated and water phase was reextracted with 20 ml of ethyl acetate. Collected organic phases were dried over Na2SO4, filtered and concentrated under reduced pressure to approximately 15g of oily residue. To this residue 15 ml of ethyl acetate were added and the mixture was cooled to 20 C and stirred at this temperature for 2h, and then cooled under 0C and stirred at this temperature for 1hour. The product was filtered off and washed with 5 ml of fresh ethyl acetate and dried. Yield: 7.55 g (90%). HPLC: 99.81 % of the product, all individual impurities under 0.10%.

144690-92-6 Triphenyl methyl olmesartan 19036162, aDioxole compound, is more and more widely used in various.

Reference£º
Patent; Krka Tovarna Zdravil, D.D., Novo Mesto; EP2334668; (2011); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem