HRID476776
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
- 6 °C
PROCEDURE
实验过程
To a solution of ethyl 2-(3-chloro-2,4,5-trifluorobenzoyl)-3-cyclopropylaminoacrylate in 40 ml of dry t-butanol is added a slurry of 1.20 g (10.7 mmol) of potassium t-butoxide in 20 ml of dry t-butanol. The reaction mixture is stirred at 6° C. for eight hours, then cooled to room temperature and concentrated. The residue is dissolved in chloroform, washed with water, dried over magnesium sulfate, filtered, and concentrated to give a pale brown solid. The crude product is purified by silica gel chromatography, and eluted with 80:20 chloroform:ethyl acetate to give 1.2 g of the title compound.
WORKUP
后处理
- temperaturecooled to room temperature
- concentrationconcentrated
- dissolutionThe residue is dissolved in chloroform
- washwashed with water
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto give a pale brown solid
- customThe crude product is purified by silica gel chromatography
- washeluted with 80:20 chloroform