HRID877154

反应详情

EQUATION

反应方程式

HRID 877154 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

8.34 g (43.29 mmol) of N′-(chloroacetyl)-2,2-dimethylpropanehydrazide were dissolved in 800 ml of dry DMF, and 4.24 g (50.52 mmol) of sodium bicarbonate were added. The reaction mixture was heated at 100° C. overnight. After cooling, the solvent was removed on a rotary evaporator, water was added to the residue and the mixture was acidified with 1 N hydrochloric acid. The mixture was extracted three times with ethyl acetate, and the combined organic phases were washed with water, dried over sodium sulfate and concentrated on a rotary evaporator. This gave 5.05 g of the target compound. The crude product was reacted further without further purification.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe solvent was removed on a rotary evaporator, water
  3. additionwas added to the residue
  4. extractionThe mixture was extracted three times with ethyl acetate
  5. washthe combined organic phases were washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated on a rotary evaporator
  8. customThe crude product was reacted further without further purification