HRID1739471

反应详情

EQUATION

反应方程式

HRID 1739471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A suspension of 2,3-dihydroxybenzaldehyde (15 g, 109 mmole) in CH2Cl2 (70 ml) was cooled to -10° C. Triethyl amine (5.49 g, 54.3 mmol) was added followed by pivaloyl chloride (6.49 g, 53.9 mmol). The reaction was allowed to stir for 1 hour at -10° C. and then warmed to ambient temperature. The reaction mixture was stirred at ambient temperature overnight, then washed with water, 1N aqueous HCl, saturated aqueous NaHCO3 and water. The organic phase was dried (MgSO4) and evaporated. The residue was purified by chromatography (eluant: ethyl acetate/hexane) to give 2-hydroxy-3-pivaloyloxybenzaldehyde: (10.15 g, 84%).

WORKUP

后处理

  1. temperaturewarmed to ambient temperature
  2. stirringThe reaction mixture was stirred at ambient temperature overnight
  3. washwashed with water, 1N aqueous HCl, saturated aqueous NaHCO3 and water
  4. dry with materialThe organic phase was dried (MgSO4)
  5. customevaporated
  6. customThe residue was purified by chromatography (eluant: ethyl acetate/hexane)