反応 #2328971

反応方程式

6-hydroxy-2-naphthoic acid

2,6-dihydroxynaphthalene

p-toluenesulfonic acid monohydrate

→

6-hydroxynaphthyl 6-hydroxy-2-naphthoate

収率 66.0%

溶媒

toluene

反応条件

後処理

1. 1
   温度was heated
2. 2
   ろ過filtered
3. 3
   ろ過the solid was finally filtered off

実験手順

A mixture of 9.41 g (0.05 mol) of 6-hydroxy-2-naphthoic acid, 24.03 g (0.15 mol) of 2,6-dihydroxynaphthalene, 0.8 g of p-toluenesulfonic acid monohydrate and 3 drops of concentrated sulfuric acid in 100 ml of toluene was heated under reflux with occasional addition of concentrated sulfuric acid (3 drops every 3 h) for 12 h. The resulting suspension was cooled to room temperature and filtered. The filtercake was suspended in methanol, the suspension was stirred for 3 h and the solid was finally filtered off. 10.9 g of 6-hydroxynaphthyl 6-hydroxy-2-naphthoate (“NpNp”) were obtained as a brownish solid which was processed in the subsequent step without further purification.

出典