HRID1094500

反应详情

EQUATION

反应方程式

HRID 1094500 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
62 °C

PROCEDURE

实验过程

A suspension of 6.56 g (40 mMol) 2-amino-4,6-dichloropyrimidine and 7.52 g (40 mMol) 6-hydroxy-1-naphthoic acid in 160 ml acetone and 80 ml 1 N aqueous NaOH is heated to 62° C. for 36 h. The mixture is cooled to rt, partially concentrated in vacuo and the residue poured into 1.6 l icewater. Under vigorous stirring, 20 ml 2 N HCl are added dropwise (pH≈4). After stirring the suspension for 30 min, the title compound is filtered off and washed with water; HPLC: tRet=12.8.

WORKUP

后处理

  1. temperatureThe mixture is cooled to rt
  2. concentrationpartially concentrated in vacuo
  3. additionthe residue poured into 1.6 l icewater
  4. additionUnder vigorous stirring, 20 ml 2 N HCl are added dropwise (pH≈4)
  5. filtrationthe title compound is filtered off
  6. washwashed with water