HRID64899

反应详情

EQUATION

反应方程式

HRID 64899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

83.3 Grams (0.324 mole) of 2-tert-butyl-3-(4-chlorophenyl)-3-hydroxypropionic acid and 125 g (0.77 mole) of 1,1'-carbonyldiimidazole were mixed with 700 ml of tetrahydrofuran, and the mixture was heated under reflux for 3 hours with stirring. After concentrating the reaction solution under reduced pressure, water and then diethyl ether were added to the residue which was then washed with water. The ether layer was separated and concentrated to form crystals with a small amount of ether left in the system. The crystal was filtered off and washed with a small amount of ether to obtain 50.6 g (38.5%) of N-{2-tert-butyl-3-(4-chlorophenyl)-3-(1-imidazolylcarbonyloxy)propanoyl}-imidazole. m.p., 69°-71° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. concentrationAfter concentrating the reaction solution under reduced pressure, water
  4. additiondiethyl ether were added to the residue which
  5. washwas then washed with water
  6. customThe ether layer was separated
  7. concentrationconcentrated
  8. customto form crystals with a small amount of ether
  9. waitleft in the system
  10. filtrationThe crystal was filtered off
  11. washwashed with a small amount of ether