反応式
[CH2:1]1[C@H:5]2[C:6](=[O:16])[NH:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10](=[O:11])[N:4]2[CH2:3][CH2:2]1.[H-].[Na+].[CH3:19]I.O>CN(C=O)C>[CH3:19][N:7]1[C:8]2[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=2[C:10](=[O:11])[N:4]2[CH2:3][CH2:2][CH2:1][CH:5]2[C:6]1=[O:16]参加物
6
実験手順
To (S)-(+)-2,3-dihydro-1H-pyrrolo[2,1-c][1,4]benzodiazapine-5,11(10H,11aH)-dione (9.9 g, 45.8 mmol) in DMF (150 ml) at 0° C. was added NaH (2.0 g, 50.4 mmol). The mixture was warmed to room temperature and stirred for 1 h before methyl iodide (8.56 ml, 137 mmol) was added dropwise. After stirring for an additional 1 h, the mixture was dumped into water (1 l) and extracted with ethyl acetate (3×100 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to a solid which was recrystallized from ethyl acetate-hexane (5.7 g, 54%), m.p. 118-120° C.
後処理
- additionwas added dropwise
- extractionextracted with ethyl acetate (3×100 ml)
- washThe combined extracts were washed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated to a solid which
- customwas recrystallized from ethyl acetate-hexane (5.7 g, 54%), m.p. 118-120° C.
出典と根拠
- ORDレコード
- ord-add530bef09548b99c9da6a84f960e5d
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05929085
関連ノート
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