反応式
[CH3:1][N:2]=[C:3]=[O:4].[NH:5]([C:7]1[CH2:8][N:9]=[C:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:25])[C:11]2[CH:16]=[C:15]([CH2:17][CH3:18])[S:14][C:12]=2[N:13]=1)[NH2:6]>O1CCCC1>[CH3:1][NH:2][C:3](=[O:4])[NH:6][NH:5][C:7]1[CH2:8][N:9]=[C:10]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[Cl:25])[C:11]2[CH:16]=[C:15]([CH2:17][CH3:18])[S:14][C:12]=2[N:13]=1参加物
4
実験手順
1.1 ml of methyl isocyanate is added to a suspension of 5 g of 2-hydrazino-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e] [1,4] diazepine in 100 ml of tetrahydrofuran, and the resulting mixture is stirred at room temperature for 2 hours. Then the reaction mixture is poured into ice water, and the precipitated crystals are collected by filtration, washed with water, dried, and recrystallized from a mixture of chloroform and ligroin to give 2-(4-methylsemicarbazido)-5-o-chlorophenyl-7-ethyl-3H-thieno[ 2,3-e][1,4]diazepine, melting at 213°-215° C.
後処理
- filtrationthe precipitated crystals are collected by filtration
- washwashed with water
- customdried
- customrecrystallized from a mixture of chloroform and ligroin
出典と根拠
- ORDレコード
- ord-cbbed60c63024bfaaa743c0aa051ec72
- 出典データセット
- uspto-grants-1976_06
- 特許番号
- US03965111
関連ノート
読み込み中…