HRID2166911

反应详情

EQUATION

反应方程式

HRID 2166911 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 700 ml of dimethylformamide, 249 g (1.22 mol) of 1,4-dihydroxy-2-naphthoic acid was added, and the mixture was stirred under a nitrogen atmosphere. To the mixture, 490 ml (2.44 mols) of a 28% solution of sodium methoxide in methanol was added dropwise over 20 minutes. After 10 minutes, 150 g (1.22 mol) of ethyl chloroacetate was added dropwise over 30 minutes, and the mixture was stirred for 3 hours while keeping the temperature at 50° C. The reaction solution was poured into a mixture of 160 ml of concentrated chloric acid and 5 l of iced water, and the precipitated crystals were filtered off and dried to obtain 335 g (95% yield) of 1-hydroxy-4-ethoxycarbonylmethyloxy-2-naphthoic acid.

WORKUP

后处理

  1. stirringthe mixture was stirred for 3 hours
  2. customat 50° C
  3. filtrationthe precipitated crystals were filtered off
  4. customdried