HRID260736

反应详情

EQUATION

反应方程式

HRID 260736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of crude 2-n-butyl-5-acetoxymethyl-1-(2-chlorophenyl)methyl-1H-imidazole (250 g) in methanol (200 mL) was treated with 10% sodium hydroxide solution (700 mL), and the mixture was heated on a steam bath for 4 hours. After cooling, methylene chloride was added, the organic phase was separated, washed with water, dried and concentrated. The residue was dissolved in ether, cooled, and seeded to give the crude product. Recrystallization from ethyl acetate gave 176 g of 2-n-butyl-1-(2-chlorophenyl)methyl-5-hydroxymethyl-1H-imidazole; mp 86°-88° C. This material was identical in all respects to the product prepared by Method A.

WORKUP

后处理

  1. temperaturethe mixture was heated on a steam bath for 4 hours
  2. temperatureAfter cooling
  3. customthe organic phase was separated
  4. washwashed with water
  5. customdried
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in ether
  8. temperaturecooled
  9. customto give the crude product
  10. customRecrystallization from ethyl acetate