HRID1065087

反应详情

EQUATION

反应方程式

HRID 1065087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureheated
  2. temperatureunder reflux for 6 h
  3. temperatureAfter cooling
  4. stirringthe mixture was shaken
  5. customThe organic layer was separated
  6. extractionwas then extracted with ether (3×100 ml)
  7. washwashed with water (1×20 ml) and with sodium carbonate solution (20 ml, 10% w/v)
  8. dry with materialthe ether solution was then dried (MgSO4)
  9. concentrationThe ether solution was concentrated under reduced pressure
  10. customto give a solid, which
  11. customwas recrystallised from aqueous ethanol