Methyl chloroformate → [2-(3-Chloro-phenyl)-1-methyl-ethyl]-carbamic acid methyl ester
反応式
Cl[C:2]([O:4][CH3:5])=[O:3].[Cl:6][C:7]1[CH:8]=[C:9]([CH2:13][CH:14]([NH2:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>C1COCC1>[CH3:5][O:4][C:2](=[O:3])[NH:16][CH:14]([CH3:15])[CH2:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([Cl:6])[CH:8]=1参加物
5
実験手順
At 0° C., methyl chloroformate (0.67 g, 7.1 mmol) was added dropwise to a mixture of 2-(3-chloro-phenyl)-1-methyl-ethylamine (1.0 g, 5.9 mmol) and potassium carbonate (1.63 g, 11.8 mmol) in THF (20 mL). After the addition, the mixture was stirred at room temperature overnight. After filtration and evaporation of the volatiles, the crude product was purified by flash column chromatography (silica gel, 12 g, 50% hexane in dichloromethane) to give the title compound as a white solid (1.2 g, 90%). MS: 228.1 (M+H+).