반응식
ClC.[F:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[NH:11][CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:25]([S:27](Cl)(=[O:29])=[O:28])[CH3:26].C(=O)(O)[O-].[Na+]>>[F:3][C:4]1[CH:9]=[C:8]([F:10])[CH:7]=[CH:6][C:5]=1[N:11]([CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)[S:27]([CH2:25][CH3:26])(=[O:29])=[O:28]참가 물질
5
실험 절차
A 4.4 g. portion of 3-(2,4-difluorophenylaminomethyl)pyridine chloromethane, and 4.1 g. of potassium carbonate and 3.9 g. of ethanesulfonyl chloride were added. The mixture was stirred under reflux for several days. It was then diluted with 20 ml. of aqueous sodium bicarbonate and 20 ml. of dichloromethane, and the organic phase was dried and evaporated to an oil. The oil was dissolved in dichloromethane and chromatographed over silica gel, eluting with dichloromethane, to obtain 1.2 g. of the desired product, after triturating with diethyl ether and petroleum ether. M.P. 91°-92°.
후처리
- temperatureunder reflux for several days
- additionIt was then diluted with 20 ml
- dry with materialof dichloromethane, and the organic phase was dried
- customevaporated to an oil
- dissolutionThe oil was dissolved in dichloromethane
- customchromatographed over silica gel
- washeluting with dichloromethane
- customto obtain 1.2 g
- customof the desired product, after triturating with diethyl ether and petroleum ether
출처 및 근거
- ORD 기록
- ord-591049fea23340ada6543bf107c543b7
- 출처 데이터셋
- uspto-grants-1989_10
- 특허 번호
- US04874775
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