HRID515269

反应详情

EQUATION

反应方程式

HRID 515269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Aminophenol (18.33 mmol, 2 g) and 4-nitrophenyl carbonochloridate (18.33 mmol, 3.69 g) in dichloromethane (10 mL) were stirred at room temperature for 30 minutes. Cyclopropylmethanamine (36.7 mmol, 3.72 mL, 2.61 g) was added followed triethylamine (55.0 mmol, 7.66 mL, 5.56 g). The reaction was allowed to stir at room temperature overnight. The reaction mixture was diluted with dichloromethane/saturated sodium hydrogen carbonate solution and filtered through a hydrophobic frit. The organic layer was concentrated and the residue was purified by silica column chromatography (eluent: 2-8% methanol in dichloromethane) to give the title compound (1.4 g). MS (ESI) m/z 207.1 [M+H]+

WORKUP

后处理

  1. filtrationfiltered through a hydrophobic frit
  2. concentrationThe organic layer was concentrated
  3. customthe residue was purified by silica column chromatography (eluent: 2-8% methanol in dichloromethane)