HRID1610952

反应详情

EQUATION

反应方程式

HRID 1610952 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oxone (Trade mark; potassium peroxymonosulfate: 28.8 g) was added to a suspension of 4-[4-[2-[(methylthio)methyl]-1H-imidazol-1-yl]butyl]phenol (8.64 g) in methanol-water (2:1) (150 ml) at 0° C. and the mixture was stirred at room temperature for 3.5 hr. The reaction mixture was adjusted to pH 6 by addition of 4N aqueous sodium hydroxide solution to precipitate crystals, which were collected by filtration. The crystals were dissolved in ethyl acetate-methanol (1:4), and the insoluble was filtered off. The filtrated was concentrated and recrystallized from ethyl acetate-methanol-hexane to give the titled compound (6.53 g) as colorless needle crystals.

WORKUP

后处理

  1. customto precipitate crystals, which
  2. filtrationwere collected by filtration
  3. dissolutionThe crystals were dissolved in ethyl acetate-methanol (1:4)
  4. filtrationthe insoluble was filtered off
  5. concentrationThe filtrated was concentrated
  6. customrecrystallized from ethyl acetate-methanol-hexane