Methyl chloroformate → (2-Cyclopropylcarbamoyl-phenyl)-carbamic acid methyl ester
反応式
[NH2:1][C:2]1[CH:13]=[CH:12][CH:11]=[CH:10][C:3]=1[C:4]([NH:6][CH:7]1[CH2:9][CH2:8]1)=[O:5].[CH3:14][O:15][C:16](Cl)=[O:17]>O>[CH3:14][O:15][C:16](=[O:17])[NH:1][C:2]1[CH:13]=[CH:12][CH:11]=[CH:10][C:3]=1[C:4](=[O:5])[NH:6][CH:7]1[CH2:8][CH2:9]1参加物
4
実験手順
To a slurry of 2-amino-N-cyclopropyl-benzamide (6.7 g, 38.1 mmol) in water was added KHCO3 (9.5 g, 95.1 mmol) followed by careful addition of methylchloroformate (5.88 ml, 76.2 mmol). The mixture was stirred for 12 h then the aqueous layer was extracted with EtOAc. The EtOAc extract was washed with 1N HCl then dried over MgSO4 and concentrated to give 8.9 g (99%) of (2-cyclopropylcarbamoyl-phenyl)-carbamic acid methyl ester.
後処理
- extractionthe aqueous layer was extracted with EtOAc
- extractionThe EtOAc extract
- washwas washed with 1N HCl
- dry with materialthen dried over MgSO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-3a9f0fe3b0a84313a213da891b71d62b
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06919331B2
反応ノート
読み込み中…