HRID2110961

反应详情

EQUATION

反应方程式

HRID 2110961 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of triflic anhydride (1.77 ml, 10.5 mmol) in dichloromethane 10 ml) was added to a mixture of 2,4-dihydroxybenzaldehyde (1.38 g, 10 mmol) and pyridine (0.85 ml, 10.5 mmol) in dichloromethane (30 ml) at −70 C. Dry ice bath was removed and the reaction mixture was stirred for 2 h at room temperature. The reaction mixture was diluted with dichloromethane, washed with water, brine and evaporated in vacuo. The crude product was purified by column chromatography (silica gel, EA:Hex, 1:6) to give 1.55 g of trifluoro-methanesulfonic acid 4-formyl-3-hydroxy-phenyl ester (57%).

WORKUP

后处理

  1. customDry ice bath was removed
  2. additionThe reaction mixture was diluted with dichloromethane
  3. washwashed with water, brine
  4. customevaporated in vacuo
  5. customThe crude product was purified by column chromatography (silica gel, EA:Hex, 1:6)