HRID1747

反应详情

EQUATION

反应方程式

HRID 1747 的结构方程式

PROCEDURE

实验过程

40.4 g (360 mmol) of potassium tert-butylate were added in portions to 60 ml of trifluoroethanol, while stirring and cooling, and the mixture was heated to 80°-90° C. After cooling, 14.4 g (70 mmol) of 4,5-dichloro-2-nitrotoluene were added and the mixture was stirred at 105° C. for 1 hour. It was concentrated in vacuo and the residue was treated with 300 ml of water to give, after filtration with suction, 12 g of crude product, which were purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.

WORKUP

后处理

  1. temperaturecooling
  2. temperaturethe mixture was heated to 80°-90° C
  3. temperatureAfter cooling
  4. stirringthe mixture was stirred at 105° C. for 1 hour
  5. concentrationIt was concentrated in vacuo
  6. additionthe residue was treated with 300 ml of water
  7. customto give
  8. filtrationafter filtration with suction, 12 g of crude product, which
  9. customwere purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.