HRID1251863

反应详情

EQUATION

反应方程式

HRID 1251863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triflic anhydride (170 ml; 1.01 mol) was added to a solution of methyl 2-hydroxy-4-methylbenzoate (153 g; 0.92 mol) in pyridine (1.5 l), at 0° C., The mixture was stirred at ambient temperature overnight. After evaporation of the pyridine, the residue was acidified to pH 3.5 with 6N HCl and extracted with ether. The organic phase was evaporated and the residue purified by flash column chromatography eluting with a gradient of 0-5% ethyl acetate/petroleum ether to give methyl 2-trifluoromethylsulfonyloxy-4-methylbenzoate (245 g; 90%).

WORKUP

后处理

  1. customAfter evaporation of the pyridine
  2. extractionextracted with ether
  3. customThe organic phase was evaporated
  4. customthe residue purified by flash column chromatography
  5. washeluting with a gradient of 0-5% ethyl acetate/petroleum ether