HRID2229253

反应详情

EQUATION

反应方程式

HRID 2229253 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(1H-imidazol-1-yl)-1-(2-naphthyl)-1-butanol (0.450 g) and p-toluenesulfonic acid hydrate (0.589 g) in dimethoxyethane (20 ml) was refluxed for 16 hours. To the mixture was added water, then the whole was concentrated and extracted with ethyl acetate. The extract was washed with water and brine, dried and concentrated. The residue was chromatographed on silica gel (ethyl acetate-MeOH=20:1) followed by crystallization from ethyl acetate-hexane to give the titled compound (0.112 g) as a colorless powder.

WORKUP

后处理

  1. temperaturewas refluxed for 16 hours
  2. concentrationthe whole was concentrated
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water and brine
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on silica gel (ethyl acetate-MeOH=20:1)
  8. customfollowed by crystallization from ethyl acetate-hexane