HRID1730359

反应详情

EQUATION

反应方程式

HRID 1730359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1,1,3,4,4,6-Hexamethyl-7-acetyl-1,2,3,4-tetrahydronaphthalene(33 g.) in 40 ml. glacial acetic acid was treated slowly with 20 g. bromine. Warming was necessary to initiate the reaction, evidenced by disappearance of the red colouration. When all the bromine had been added,the mixture was cooled and poured onto ice to give a pale green gum. The whole was extracted with ether, the ethereal extracts washed with dilute Na2CO3, water and finally dried over MgSO4. Evaporation ofthe ether gave a pale green solid which was recrystallised from EtOH to give the title compound 27.6 g. (64%), m.p. 68° C. Analysis : Calculated for C18H25OBr, C, 64.09%; H, 7.47%. Found : C, 64.40%; H, 7.65%.

WORKUP

后处理

  1. temperatureWarming
  2. customthe reaction
  3. temperaturewas cooled
  4. additionpoured onto ice
  5. customto give a pale green gum
  6. extractionThe whole was extracted with ether
  7. washthe ethereal extracts washed with dilute Na2CO3, water
  8. dry with materialfinally dried over MgSO4
  9. customEvaporation ofthe ether
  10. customgave a pale green solid which
  11. customwas recrystallised from EtOH