HRID354726

反应详情

EQUATION

反应方程式

HRID 354726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4.32 G (0.02 Mol) of the compound of Example 4, 0.1 g of Aliquat 336, 3.9 g of t-butyl bromoacetate, 50 ml of hexane, 10 g of sodium hydroxide and 24 ml of water was held at reflux for 1 hour. The reaction mixture was filtered. The hexane layer was separated, dried over MgSO4 and concentrated under reduced pressure. The residue (1.6 g) was chromatographed on silica gel using ether-petroleum ether (2:98 v/v) as eluant. The first fraction gave 1.1 g (16.5%) of t-butyl{[2-chloro-4-(trifluoromethyl)-5-thiazolyl]methoxy}acetate, as an oil, nD25 1.4607.

WORKUP

后处理

  1. temperatureat reflux for 1 hour
  2. filtrationThe reaction mixture was filtered
  3. customThe hexane layer was separated
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customThe residue (1.6 g) was chromatographed on silica gel