반응 #50926

반응 방정식

sodium hydrogensulfite

sodium carbonate

2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide

OXONE

→

title compound

수율 93.0%

2-(3,5-Bis-trifluoromethyl-phenyl)-N-[6-(1,1-dioxo-1λ6-thiomorpholin-4-yl)-4-o-tolyl-pyridin-3-yl]-N-methyl-isobutyramide

수율 93.0%

용매

methanol

반응 조건

후처리

1. 1
   기타methanol was removed in vacuo
2. 2
   workup.ADDITIONThe residue was diluted with 25 ml water
3. 3
   추출extracted with three 25-ml portions of dichloromethane
4. 4
   건조The combined organic layers were dried (sodium sulfate)
5. 5
   기타purified by flash chromatography
6. 6
   기타crystallized from ethanol

실험 절차

To a solution of 1.00 g (1.72 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-methyl-N-(6-thiomorpholin-4-yl-4-o-tolyl-pyridin-3-yl)-isobutyramide in 10 ml methanol were added 1.59 g (2.58 mmol) OXONE®. After stirring for 2 days at room temperature, 5 ml 38% sodium hydrogensulfite solution and 20 ml saturated sodium carbonate solution were added consecutively and methanol was removed in vacuo. The residue was diluted with 25 ml water and extracted with three 25-ml portions of dichloromethane. The combined organic layers were dried (sodium sulfate), purified by flash chromatography and crystallized from ethanol to give 980 mg (93%) of the title compound as white crystals. M.p. 200-201° C.

출처