HRID591188

反应详情

EQUATION

反应方程式

HRID 591188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

1-(1-(4-Chlorophenyl)cyclobutyl)-2-nitroethanol (5.2 g, 20.34 mmol) was dissolved in dichloromethane (41 ml) and trifluoroacetic acid anhydride (2.87 ml, 20.34 mmol) was added. The reaction mixture was cooled to 0° C. and triethylamine (5.67 ml, 40.7 mmol) was added dropwise. The reaction was slowly warmed to room temperature and stirring was continued for 2 h. The reaction mixture was diluted with dichloromethane and washed with aqueous hydrochloric acid (1 N). The organic layer was dried (magnesium sulfate) and concentrated in vacuo. The crude product was purified by flash chromatography (silica, dichloromethane, methanol). Yield: 3.99 g (16.79 mmol, 83%)

WORKUP

后处理

  1. temperatureThe reaction was slowly warmed to room temperature
  2. washwashed with aqueous hydrochloric acid (1 N)
  3. dry with materialThe organic layer was dried (magnesium sulfate)
  4. concentrationconcentrated in vacuo
  5. customThe crude product was purified by flash chromatography (silica, dichloromethane, methanol)