Methyl chloroformate → Methyl 2,3-dihydro-1H-indole-1-carboxylate
反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.Cl[C:11]([O:13][CH3:14])=[O:12].C(N(CC)CC)C>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH3:14][O:13][C:11]([N:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH2:2]1)=[O:12]参加物
6
実験手順
A mixture of indoline (11.97 g, 0.1 mol), methyl chloroformate (15.45 mL, 0.2 mol), triethylamine (40.4 g, 0.4 mol), and DMAP (0.5 g, 0.004 mol) in CH2Cl2 (100 mL) was stirred for 16 hours. The reaction mixture was quenched with water (10 mL). The reaction was extracted with CH2Cl2 (1×40 mL). The organic layer washed with water (1×50 mL), dried over anhydrous magnesium sulfate, filtered and the resultant filtrate was concentrated in vacuo to provide the title compound (17.6 g, 99%) which was used without further purification.
後処理
- customThe reaction mixture was quenched with water (10 mL)
- extractionThe reaction was extracted with CH2Cl2 (1×40 mL)
- washThe organic layer washed with water (1×50 mL)
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationthe resultant filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-fb6e172a4c7c470882b10a1552740b38
- 出典データセット
- uspto-grants-2004_12
- 特許番号
- US06831080B2
反応ノート
読み込み中…