HRID1030512

反应详情

EQUATION

反应方程式

HRID 1030512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 9.2 g of ethyl 6-acetoxymethylnicotinate in chloroform (40 ml) was added an ethanol solution of sodium ethoxide prepared from 0.92 g of sodium and 23 ml of ethanol, and the mixture was stirred at room temperature for 2 hours. The reaction liquid was poured into water containing 6 ml of acetic acid and the chloroform layer was separated and dried with anhydrous sodium sulfate. The solvent was removed under reduced pressure, carbon tetrachloride was added to the residue, and the insoluble substance was removed by filtration. The filtrate was concentrated under reduced pressure and the residue was recrystallized from ethyl acetate/hexane to obtain 5.1 g of ethyl 6-hydroxymethylnicotinate. ##STR8##

WORKUP

后处理

  1. customThe reaction liquid
  2. customthe chloroform layer was separated
  3. dry with materialdried with anhydrous sodium sulfate
  4. customThe solvent was removed under reduced pressure, carbon tetrachloride
  5. additionwas added to the residue
  6. customthe insoluble substance was removed by filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue was recrystallized from ethyl acetate/hexane