HRID260264

反应详情

EQUATION

反应方程式

HRID 260264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To o-xylene (Fluka purum, 905 ml, 7.5 mole), kept under stirring, at 0°, there was added AlCl3 (6.7 g, 50 mmole), and then, dropwise, tert-butyl chloride (Fluka puriss., 551 ml, 5 mole), during 1.25 h, while keeping the temperature between 0° and 5° (the evolving HCl was trapped in NaOH 2.5 N). The temperature was allowed to increase to room temperature. After 60 h, the reaction mixture was poured on a mixture of ice and ether, the organic phase was successively washed with brine (2x), H2O, sat. NaHCO3 and brine, dried over Na2SO4 and distilled under vacuum (Vigreux column, 30 cm) to provide 4-tert-butyl-1,2-dimethylbenzene (purity >99%, yield 90%).

WORKUP

后处理

  1. customthe temperature between 0° and 5°
  2. washthe organic phase was successively washed with brine (2x), H2O, sat. NaHCO3 and brine
  3. dry with materialdried over Na2SO4
  4. distillationdistilled under vacuum (Vigreux column, 30 cm)