反応式
C(Cl)(=O)[O:2][CH2:3][CH3:4].[N:7]1[C:12]2[NH:13][C:14]3[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=3[C:16](=[O:18])[NH:17][C:11]=2[CH:10]=[CH:9][CH:8]=1.[CH2:23]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])[CH3:24].[OH-].[Na+]>O1CCCC1>[CH2:23]([N:25]([CH2:28][CH:29]1[CH2:11][CH2:10][CH2:9][CH2:8][N:7]1[CH2:4][C:3]([N:13]1[C:14]2[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=2[C:16](=[O:18])[NH:17][C:11]2[CH:10]=[CH:9][CH:8]=[N:7][C:12]1=2)=[O:2])[CH2:26][CH3:27])[CH3:24]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 0 °C
実験手順
Ethyl chlorocarbonate (11.0 g, 0.101 mol) is added dropwise, at 0° C., to a suspension of 2-[(diethylamino)methyl]-1-piperidino acetic acid (22.83 g, 0.1 mol) in dry tetrahydrofuran (200 ml). Then, 5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one (21.12 g, 0.1 mol) and triethylamine (20.24 g, 0.2 mol) are added to the resulting suspension which is then stirred for a further hour at 0° C. and then for 4 hours at ambient temperature. The mixture is poured into 2N sodium hydroxide solution (1.6 liters), extracted exhaustively with dichloromethane, the organic phase concentrated to dryness and the residue purified by recrystallization from ethanol and from methanol. Colorless crystals (6.3 g) are obtained, mp. 226°-228° C., which were shown by thin layer chromatography, mixed melting point and IR spectrum to be identical to a sample prepared according to Example 34.
後処理
- extractionextracted exhaustively with dichloromethane
- concentrationthe organic phase concentrated to dryness
- customthe residue purified by recrystallization from ethanol and from methanol
出典と根拠
- ORDレコード
- ord-901753c25af7418f9c10fcb008b79f6c
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04550107
関連ノート
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