반응식
Cl.Cl[CH:3]([C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[S:22][C:23]([CH3:26])=[CH:24][CH:25]=1)[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].C(S([O-])=O)O.[Na+]>ClCCl>[CH3:8][N:6]([CH3:7])[C:4](=[O:5])[CH2:3][C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[S:22][C:23]([CH3:26])=[CH:24][CH:25]=1참가 물질
실험 절차
40 g (0.0938 mole) of α-chloro-N,N-dimethyl-2-(5-methylthien-2-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 1200 ml of dichloromethane are treated with 43.6 (0.283 mole) of Rongalite®, while stirring the mixture at room temperature for 6 h. The suspension is filtered, it is rinsed with dichloromethane and the organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10, then to neutral pH with a saturated sodium chloride solution. The organic phase is dried over sodium sulphate and the solvent is evaporated under reduced pressure. A beige-coloured solid is obtained which is purified by chromatography on a silica gel column, eluting with a 95/5 mixture of dichloromethane/methanol. 23.9 g of a white solid are obtained. Melting point: 216°-218° C.
후처리
- filtrationThe suspension is filtered
- washit is rinsed with dichloromethane
- washthe organic phase is washed (pH=1) with 500 ml of 0.5N sodium hydroxide up to a pH>10
- dry with materialThe organic phase is dried over sodium sulphate
- customthe solvent is evaporated under reduced pressure
- customA beige-coloured solid is obtained which
- customis purified by chromatography on a silica gel column
- washeluting with a 95/5 mixture of dichloromethane/methanol
출처 및 근거
- ORD 기록
- ord-edf4702c5b204ea8b368e24852d3b023
- 출처 데이터셋
- uspto-grants-1995_05
- 특허 번호
- US05418248
연결된 노트
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