成人免费xx,国产又黄又湿又刺激不卡网站,成人性视频app菠萝网站,色天天天天

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Methyl 4-(4-Fluorophenyl)-6-isopropyl-2-(methylsulfonyl)pyrimidine- 5-carboxylate
799842-06-1

Methyl 4-(4-Fluorophenyl)-6-isopropyl-2-(methylsulfonyl)pyrimidine- 5-carboxylate synthesis

5synthesis methods
160009-35-8 Synthesis
Methyl 4-(4-Fluorophenyl)-6-isopropyl-2-(methylthio)pyrimidine-5-carboxylate

160009-35-8
10 suppliers
$140.00/25mg

-

Yield:799842-06-1 90.92%

Reaction Conditions:

with ammonium peroxomolybdate;dihydrogen peroxide;Aliquat 336 in dichloromethane;water at 20 - 35; for 19 - 21.5 h;Product distribution / selectivity;

Steps:

1.B; 3.B; II

Step -B: PREPARATION OF METHYL-4- (4-FLUOROPHENYL)-6-ISOPROPYL-2-METHYL SULFONYL PYRIMIDINE-5-CARBOXYLATE (FORMULA VII) To a four neck clean RB flask, charged dichloromethane (1500.0 ml), Methyl -4- (4-fluorophenyl)-6-isopropyl-2-methylthio-pyrimidine-5-carboxylate (150.0gm,0.468 moles),ammonium heptamolybdate tetrahydrate (8.62 gm,0.00697 moles) and tricaprylyl methyl ammonium chloride (Aliquat336) (21.0 gm,0.047 moles) were stirred at 25 to 300C. This was followed by the slow addition of 50 % hydrogen peroxide solution (96.5 gm, 1.42 moles) at 20 to 350C over period of 1 to 1.5 hrs. Reaction mass were further stirred at 25 to 30 C for 18 to 20 hours. After the completion of reaction charged water (450.0 ml) and continued stirring for 10 min. This was followed by layer separation. The aqueous layer was extracted with 130.0 ml dichloromethane. Combined all organic layers and Washed with water (2 x 500.0 ml). Dichloromethane was distilled under reduced pressure at 40 to 450C and followed by degassing for 30 min at 50 to 550C under reduced pressure. Isopropyl alcohol (175.0 ml) was added and distilled out under vacuum at 50 to 55 0C, followed by the addition of isopropyl alcohol (350.0 ml) and heat to 60 to 650C to get clear solution. Cooled solution to 25 to 300C and stirred for 2.0 hrs at 25 to 300C .Further cooled to 0 to 5 0C and stirred for 2.0 hrs at 0 to 5 0C. Filtered and washed with chilled (0 0C) isopropyl alcohol (100.0 ml). The wet product was dried at 40 to 450C under reduced pressure to obtain Methyl-4- (4-fluorophenyl)-6-isopropyl-2- methylsulfonyl pyrimidine-5-carboxylate (150.0 g, 90.92%).; Step -B: PREPARATION OF METHYL-4- (4-FLUOROPHENYL)-6-ISOPROPYL-2- METHYL SULFONYL PYRIMIDINE-5-CARBOXYLATE (FORMULA VII) To a four neck clean RB flask, charged dichloromethane (2530.0ml), Methyl-4- (4-fluorophenyl)-6-isopropyl-2-methylthio-pyrimidine-5-carboxylate(225.0gm,0.7022 moles),ammonium heptamolybdate tetrahydrate (12.93 gm,.01046moles) and tricaprylyl methyl ammonium chloride (Aliquat336) (28.44 gm,0.0703 moles) were stirred at 25 to 300C. This was followed by the slow addition of 50 % hydrogen peroxide solution (145.15 gm, 2.1393 moles) at 20 tq 350C over period of 1 to 1.5 hrs. Reaction mass were further stirred at 25 to 300C for 18 to 20 hours. After the completion of reaction charged water (700.0ml) and continued stirring for 10 min. This was followed by layer separation. The aqueous layer was extracted with 330.0 ml dichloromethane. Combined all organic layers and Washed with water (2 x 750.0 ml). Dichloromethane was distilled under reduced pressure at 40 to 450C and followed by degassing for 30 min at 50 to 550C under reduced pressure. Isopropyl alcohol (225.0 ml) was added and distilled out under vacuum at 50 to 55 0C, followed by the addition of isopropyl alcohol (900.0 ml) and heat to 60 to 650C to get clear solution. Cooled solution to 25 to 300C and stirred for 2.0 hrs at 25 to 300C .Further cooled to 0 to 5 0C and stirred for 2.0 hrs at 0 to 5 0C. Filtered and washed with chilled (0 0C) isopropyl alcohol (110.0 ml). The wet product was dried at 40 to 450C under reduced pressure to obtain 213.0 gm Methyl-4- (4-fluorophenyl)-6-isopropyl-2- methylsulfonyl pyrimidine-5-carboxylate . Purity by HPLC: 98.34%Melting point : 115.9.O0C to 117.5°C

References:

WO2008/59519,2008,A2 Location in patent:Page/Page column 8; 15-16; 20

Methyl 4-(4-Fluorophenyl)-6-isopropyl-2-(methylsulfonyl)pyrimidine- 5-carboxylate Related Search: