反応式
[NH:1]([C:3]1[CH2:4][N:5]=[C:6]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[Cl:21])[C:7]2[CH:12]=[C:11]([CH2:13][CH3:14])[S:10][C:8]=2[N:9]=1)[NH2:2].[N:22]([O-])=O.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>Cl.O>[Cl:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[C:6]1[C:7]2[CH:12]=[C:11]([CH2:13][CH3:14])[S:10][C:8]=2[N:9]2[N:22]=[N:2][N:1]=[C:3]2[CH2:4][N:5]=1参加物
実験手順
[f] 10 g of 2-hydrazino-5-o-chlorophenyl-7-ethyl-3H-thieno[2,3-e][1,4]diazepine prepared in the above example [d] is suspended in 54 ml of 2N hydrochloric acid. A solution of 2.4 g of sodium nitrite in 20 ml of water is added to the suspension at -5°C with stirring. The mixture is stirred at room temperature for 30 minutes, and then alkalified with sodium carbonate. The precipitated crystals are filtered off and dissolved in chloroform, and the solution is washed with water. The chloroform layer is dried over anhydrous magnesium sulfate, and the chloroform is distilled off under reduced pressure. The reddish brown jellylike residue thus obtained is crystallized from a mixture of ligroin and ethanol to give 8.2 g of 6-o-chlorophenyl-8-ethyl-4H-tetrazolo[5,1-c]thieno[2,3-e] [1,4]diazepine as white crystals. The product, when recrystallized from ethanol, melts at 135° - 136°C.
後処理
- stirringThe mixture is stirred at room temperature for 30 minutes
- filtrationThe precipitated crystals are filtered off
- dissolutiondissolved in chloroform
- washthe solution is washed with water
- dry with materialThe chloroform layer is dried over anhydrous magnesium sulfate
- distillationthe chloroform is distilled off under reduced pressure
- customThe reddish brown jellylike residue thus obtained
- customis crystallized from a mixture of ligroin and ethanol
出典と根拠
- ORDレコード
- ord-0e4c796d5c3441c3bd35cceb2000c360
- 出典データセット
- uspto-grants-1976_04
- 特許番号
- US03952006
関連ノート
読み込み中…