Hydroxyamine hydrochloride → HCID 178526325, 화합물
반응식
[S:1]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[CH2:5][NH:4][C:3](=S)[CH2:2]1.Cl.[NH2:14][OH:15].C([O-])(=O)C.[Na+]>C(O)C>[OH:15][N:14]=[C:3]1[NH:4][CH2:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=2[S:1][CH2:2]1참가 물질
5
실험 절차
A mixture of 4,5-dihydro-1,4-benzothiazepin-3(2H)-thione (1.56 g), hydroxylamine hydrochloride (0.83 g) and sodium acetate (0.98 g) in dry ethanol (100 ml) was heated under reflux for three hours. The mixture was cooled, and the precipitated solid was collected by filtration and washed with water. Purification of the precipitate by flash chromatography using dichloromethane/ethanol (95:5) as eluent gave 3-hydroxyimino-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from ethanol. Yield 1.2 g (m.p. 208°-210° C.).
후처리
- temperaturewas heated
- temperatureunder reflux for three hours
- temperatureThe mixture was cooled
- filtrationthe precipitated solid was collected by filtration
- washwashed with water
- customPurification of the precipitate by flash chromatography
출처 및 근거
- ORD 기록
- ord-b33d00791fe9425fb413cb82aff8b2c9
- 출처 데이터셋
- uspto-grants-1996_12
- 특허 번호
- US05580866
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