Hydroxyamine hydrochloride → HCID 178526325、化合物
反応式
[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]1参加物
5
実験手順
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.).
後処理
- 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
出典と根拠
- ORDレコード
- ord-b33d00791fe9425fb413cb82aff8b2c9
- 出典データセット
- uspto-grants-1996_12
- 特許番号
- US05580866
反応ノート
読み込み中…