Water → HCID 21471776、化合物
反応式
[Cl:1][CH2:2][C:3]([C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1)=O.O>C([SiH](CC)CC)C.FC(F)(F)C(O)=O>[Cl:1][CH2:2][CH2:3][C:5]1[S:15][C:8]2[C:9](=[O:14])[NH:10][CH2:11][CH2:12][CH2:13][C:7]=2[CH:6]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
A mixture of 1.9 g of 2-chloroacetyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one in 5.4 ml of triethylsilane and 15 ml of trifluoroacetic acid was stirred at 50° C. for 12 hours. The mixture was poured into water, alkalified and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by column chromatography on a silica gel to give 0.85 g of 2-chloroethyl-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one as white crystals, m.p. 156°-158° C.
後処理
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- customdried
- concentrationconcentrated
- customThe residue was purified by column chromatography on a silica gel
出典と根拠
- ORDレコード
- ord-4d15ec676cfb411ea4a37f98e9ecc9d9
- 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…