HRID2071976

反应详情

EQUATION

反应方程式

HRID 2071976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.55 g. (9.37 mmoles) of 4,4-dimethyl-9-hydroxy-7-(4-p-fluorophenyl-1-methylbutyl)-1,2,3,4-tetrahydrocyclopenta [c] [1]benzopyran are combined with 1.82 g. (9.37 mmoles) of γ-pyrrolidinobutyric acid hydrochloride and 2.06 g. (10.0 mmoles) of dicyclohexylcarbodiimide in 150 ml. of methylene chloride and stirred at room temperature for 21/2 hours. The insoluble by-product of dicyclohexylurea is removed by filtration and the filtrate is evaporated to give a residue which crystallized upon standing. The material is triturated with ether and filtered. Recrystallization from benzene-ether gives the product as colorless crystals.

WORKUP

后处理

  1. customThe insoluble by-product of dicyclohexylurea is removed by filtration
  2. customthe filtrate is evaporated
  3. customto give a residue which
  4. customcrystallized
  5. customThe material is triturated with ether
  6. filtrationfiltered
  7. customRecrystallization from benzene-ether