HRID1873229

反应详情

EQUATION

反应方程式

HRID 1873229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Diethyl 2-(3-chloro-4-nitrophenyl)-2-methylmalonate (119 mg, 0.36 mmol.), ethyl cyanoacetate (81 mg, 0.72 mmol.), powdery potassium carbonate (119 mg, 0.86 mmol.), and dimethyl sulfoxide (1 mL) were mixed and stirred at 80° C. for 2 hours. The reaction mixture was cooled to room temperature, and washed with diethyl ether after addition of water. The aqueous portion was made acidic by addition of 6N hydrochloric acid, and extracted with diethyl ether. The ether portion was washed successively with water and an aqueous saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was distilled off to give 133 mg (yield: 92%) of the desired compound as a yellow oil.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washwashed with diethyl ether
  3. additionafter addition of water
  4. additionThe aqueous portion was made acidic by addition of 6N hydrochloric acid
  5. extractionextracted with diethyl ether
  6. washThe ether portion was washed successively with water
  7. dry with materialan aqueous saturated sodium chloride solution, and dried over anhydrous sodium sulfate
  8. distillationThe solvent was distilled off