HRID476776

反应详情

EQUATION

反应方程式

HRID 476776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled to room temperature
  2. concentrationconcentrated
  3. dissolutionThe residue is dissolved in chloroform
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto give a pale brown solid
  9. customThe crude product is purified by silica gel chromatography
  10. washeluted with 80:20 chloroform