Water → HCID 21472076、化合物
反応式
[S:1]1[C:5]2[C:6](=[O:11])[NH:7][CH2:8][CH2:9][CH2:10][C:4]=2[CH:3]=[CH:2]1.[Cl:12][CH2:13][C:14](Cl)=[O:15].[Cl-].[Al+3].[Cl-].[Cl-].O>ClCCl>[Cl:12][CH2:13][C:14]([C:2]1[S:1][C:5]2[C:6](=[O:11])[NH:7][CH2:8][CH2:9][CH2:10][C:4]=2[CH:3]=1)=[O:15]参加物
6
実験手順
To a solution of 2 g of 4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one and 2 g of chloroacetyl chloride in 25 ml of dichloromethane was added 4.8 g of aluminum chloride. The mixture was stirred for 30 minutes, refluxed under heating for an hour and then poured into water. The precipitated crystals were collected by filtration and washed with isopropyl alcohol to give 2 g of 2-chloroacetyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one, m.p. 221°-223° C. (decomposition).
後処理
- temperaturerefluxed
- temperatureunder heating for an hour
- filtrationThe precipitated crystals were collected by filtration
- washwashed with isopropyl alcohol
出典と根拠
- ORDレコード
- ord-52e62c26e2204f79892617b06b6942e6
- 出典データセット
- uspto-grants-1996_07
- 特許番号
- US05532240
反応ノート
読み込み中…