HRID607339
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
PROCEDURE
实验过程
For preparation of the silanol, 60 mmol 1-naphthyl bromide are metallized with the equimolar amount of n-butyllithium (2 M solution in cyclohexane, 60 mmol) at −20° C. in 400 ml diethyl ether and 60 mmol dichlorodiphenylsilane is then added, in accordance with Example 2.1. After addition of the dichlorodiphenylsilane, the reaction mixture is heated under reflux for 3 h and then hydrolysed by addition of water (100 g). After the organic phase which has been separated off has been washed neutral, the solution is concentrated in vacuo and the crude product is obtained as a white solid. Crude yield: 21.17 g, content: 84% (GC-MS).
WORKUP
后处理
- temperaturethe reaction mixture is heated
- temperatureunder reflux for 3 h
- customAfter the organic phase which has been separated off
- washhas been washed neutral
- concentrationthe solution is concentrated in vacuo