反应 #160905

反应方程式

catechol

adamantane diol

Water

→

product

1,3 bis(3,4 dihydroxyphenyl)adamantane

溶剂

methanesulfonic acid

反应条件

后处理

1. 1
   萃取the mixture extracted into 10% methanol in chloroform which
2. 2
   其他was dried
3. 3
   其他evaporated in vacuo
4. 4
   其他to give a white solid
5. 5
   其他Purification by column chromatography over silica gel eluting with 0-20% methanol in chloroform

实验过程

According to the method described by Lu a solution of catechol (1.0 g) and adamantane diol (0.5 g) in methanesulfonic acid (2 ml) was heated to 80° C. for 3 hours, then left at room temperature overnight. Water was added and the mixture extracted into 10% methanol in chloroform which was dried and evaporated in vacuo to give a white solid. Purification by column chromatography over silica gel eluting with 0-20% methanol in chloroform gave the product as a white solid. Crystallisation from diethyl ether/40% petroleum ether then gave the pure product 10 as a white crystalline solid (210 mg, 20%).

来源