HRID839773

反应详情

EQUATION

反应方程式

HRID 839773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 50 grams of 2,6-di tert.butyl-4-(α-hydroxyethyl)phenol in 100 milliliters of hexane was stirred vigorously with 100 milliliters of concentrated HCl for 1 hour. The hexane layer was separated and the hexane removed by distillation under aspirator vacuum. The residual 2,6-di tert.butyl-4-(α-chloroethyl)phenol was dissolved in 100 milliliters of pyridine and the solution was heated under reflux for 30 minutes. Pyridine was removed by distillation under aspirator vacuum and the residue, after washing with water, was crystallized from acetone at -78° C. There was obtained 44 grams of product with a melting point of 36°-39° C.

WORKUP

后处理

  1. customThe hexane layer was separated
  2. customthe hexane removed by distillation under aspirator vacuum
  3. dissolutionThe residual 2,6-di tert.butyl-4-(α-chloroethyl)phenol was dissolved in 100 milliliters of pyridine
  4. temperaturethe solution was heated
  5. temperatureunder reflux for 30 minutes
  6. customPyridine was removed by distillation under aspirator vacuum
  7. washthe residue, after washing with water
  8. customwas crystallized from acetone at -78° C