HRID1747
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturecooling
- temperaturethe mixture was heated to 80°-90° C
- temperatureAfter cooling
- stirringthe mixture was stirred at 105° C. for 1 hour
- concentrationIt was concentrated in vacuo
- additionthe residue was treated with 300 ml of water
- customto give
- filtrationafter filtration with suction, 12 g of crude product, which
- customwere purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.