反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
A mixture of 9.46 g of 3-(5-chloropentyl)-4-methyl-2,5-furandione and 8.13 g of 4-amino-2-(trifluoromethyl)benzonitrile in 22 ml of ethanol was mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it was stirred for 2 days at 90° C. For working-up, the molecular sieve was filtered off after cooling, washed with ethanol, and the combined ethanol solutions were concentrated by evaporation. The residue was taken up in ethyl acetate and washed with water as well as saturated sodium chloride solution. After drying on sodium sulfate and concentration by evaporation, it was chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound was thus obtained as a white solid.
WORKUP
后处理
- additionwas mixed under a nitrogen atmosphere with 2.5 g of an activated molecular sieve (0.3 nm), and it
- filtrationthe molecular sieve was filtered off
- temperatureafter cooling
- washwashed with ethanol
- concentrationthe combined ethanol solutions were concentrated by evaporation
- washwashed with water as well as saturated sodium chloride solution
- customAfter drying on sodium sulfate and concentration by evaporation, it
- customwas chromatographed on silica gel with ethyl acetate/hexane/toluene, and 11.69 g of the title compound
- customwas thus obtained as a white solid