HRID486421

反应详情

EQUATION

反应方程式

HRID 486421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

Next, 2,5-dimethyl-2,5-dichlorohexane (183 g, 1 mol) is stirred with 3-ethylphenol (146.4 g, 1.2 mol) and aluminum chloride (4 g) is added. The mixture is heated at 95° C., with stirring, for 1.5 hr, after which ethylene dichloride (100 ml) is added, and then the heating continued. After 1 hr, the mixture is cooled to 20° C., and poured onto an ice water/hydrochloric acid mixture (150 ml, 10% HCl solution). The mixture is then extracted with toluene (500 ml), the organic layer separated, washed with brine (3×50 ml) and dried (Na2SO4). The solvent is removed by distillation and the residue crystallized from a hexane/benzene solvent mixture to give 7-ethyl-1,1,4,4-tetramethyl-5-hydroxy-1,2,3,4-tetrahydronaphthalene.

WORKUP

后处理

  1. additionis added
  2. waitAfter 1 hr
  3. temperaturethe mixture is cooled to 20° C.
  4. extractionThe mixture is then extracted with toluene (500 ml)
  5. customthe organic layer separated
  6. washwashed with brine (3×50 ml)
  7. dry with materialdried (Na2SO4)
  8. customThe solvent is removed by distillation
  9. customthe residue crystallized from a hexane/benzene solvent mixture