(-)-1-(N-methylanthraniloyl)-proline → 10-methyl-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H,11aH)-dione
反応式
[CH3:1][NH:2][C:3]1[C:4](=[CH:15][CH:16]=[CH:17][CH:18]=1)[C:5]([N:7]1[CH2:14][CH2:13][CH2:12][C@H:8]1[C:9](O)=[O:10])=[O:6]>O1CCCC1>[CH3:1][N:2]1[C:3]2[CH:18]=[CH:17][CH:16]=[CH:15][C:4]=2[C:5](=[O:6])[N:7]2[CH2:14][CH2:13][CH2:12][CH:8]2[C:9]1=[O:10]参加物
3
実験手順
A mixture of 24.8 g. of racemic 1-(N-methylanthraniloyl)proline and 21 g. of dicyclohexylcarbonyl diimide in 300 ml. of tetrahydrofuran is stirred at room temperature for 24 hours and then heated on the steam bath for 4 hours. The reaction mixture is filtered to remove the insoluble dicyclohexyl urea and the mother liquid is concentrated to recover the desired product, which is further purified by recrystallization from ethyl acetate.
後処理
- additionA mixture of 24.8 g
- temperatureheated on the steam bath for 4 hours
- filtrationThe reaction mixture is filtered
- customto remove the insoluble dicyclohexyl urea
- concentrationthe mother liquid is concentrated
- customto recover the desired product, which
- customis further purified by recrystallization from ethyl acetate
出典と根拠
- ORDレコード
- ord-6860e4264a474dbc89fdcdd0f4faeb94
- 出典データセット
- uspto-grants-1976_07
- 特許番号
- US03968230
反応ノート
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