HRID1094500
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture is cooled to rt
- concentrationpartially concentrated in vacuo
- additionthe residue poured into 1.6 l icewater
- additionUnder vigorous stirring, 20 ml 2 N HCl are added dropwise (pH≈4)
- filtrationthe title compound is filtered off
- washwashed with water