HRID1978912

反应详情

EQUATION

反应方程式

HRID 1978912 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

13.6 g (83 mmol) of carbonyldiimidazole are added to 33.0 g (83 mmol) of 4-(2-chloro-6-fluorophenyl)-3-cyclopentyloxycarbonyl-1,4-dihydro-2,6-dimethylpyridine-5-carboxylic acid in 350 ml of tetrahydrofuran and the mixture is heated to reflux for 3 h. Thin-layer chromatographic checking (silica gel, toluene/ethyl acetate 1:1) shows complete reaction, after which the reaction mixture is concentrated, the residue is taken up in ethyl acetate, and the solution is washed twice with water, dried over sodium sulphate and concentrated again. The target compound precipitates from ether in the form of white crystals of m.p. 150° C.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 3 h
  3. customreaction
  4. concentrationafter which the reaction mixture is concentrated
  5. washthe solution is washed twice with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated again
  8. customThe target compound precipitates from ether in the form of white crystals of m.p. 150° C.