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
A mixture of hydrobromic acid (26.2 g, 48%), concentrated sulphuric acid (10.82 g), and 2-(adamantan-1-yl)ethanol (10.82 g, 0.06 mol) was stirred and heated under reflux for 6 h. After cooling, water (60 ml) was added to the reaction mixture and the mixture was shaken. The organic layer was separated, and was then extracted with ether (3×100 ml). The extracts were combined, washed with water (1×20 ml) and with sodium carbonate solution (20 ml, 10% w/v) and the ether solution was then dried (MgSO4). The ether solution was concentrated under reduced pressure to give a solid, which was recrystallised from aqueous ethanol, to afford 1-(adamantan-1-yl)-2-bromoethane as white plates, m.p. 71°-72°.
WORKUP
后处理
- temperatureheated
- temperatureunder reflux for 6 h
- temperatureAfter cooling
- stirringthe mixture was shaken
- customThe organic layer was separated
- extractionwas then extracted with ether (3×100 ml)
- washwashed with water (1×20 ml) and with sodium carbonate solution (20 ml, 10% w/v)
- dry with materialthe ether solution was then dried (MgSO4)
- concentrationThe ether solution was concentrated under reduced pressure
- customto give a solid, which
- customwas recrystallised from aqueous ethanol