L-Proline → HCID 56977087、化合物
反応式
[CH2:1]([C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[NH:13][C:12](=[O:14])[O:11][C:9](=O)[C:8]=12)[CH3:2].[NH:15]1[CH2:22][CH2:21][CH2:20][C@H:16]1C(O)=O>CS(C)=O>[CH2:1]([C:3]1[C:8]2[C:9](=[O:11])[N:15]3[CH2:22][CH2:21][CH2:20][C@H:16]3[C:12](=[O:14])[NH:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)[CH3:2]参加物
4
実験手順
7.65 g (0.04 mol) of 6-ethylisatoic acid anhydride and 4.6 g (0.04 mol) of L-proline are suspended in 40 ml of dimethyl sulphoxide, heated to 70° for 2.5 hours, the solvent is removed in a high vacuum and the oil obtained is heated to 170° for 15 minutes. The crude product is purified by chromatography on silica gel using chloroform for the elution. There is obtained amorphous (S)-6-ethyl-1,2,3,11a-tetrahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione.
後処理
- temperatureheated to 70° for 2.5 hours
- customthe solvent is removed in a high vacuum
- customthe oil obtained
- temperatureis heated to 170° for 15 minutes
- customThe crude product is purified by chromatography on silica gel
- washfor the elution
出典と根拠
- ORDレコード
- ord-81b317b17d834741bb2ff2d15d091890
- 出典データセット
- uspto-grants-1982_10
- 特許番号
- US04353827
反応ノート
読み込み中…