HRID1094295

反应详情

EQUATION

反应方程式

HRID 1094295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 4-bromo-2,6-dimethyl-phenol (20.1 g, 100 mmol) and allylchloride (32.7 g, 428 mmol) in 3 N aq. NaOH (100 mL) and isopropanol (250 mL) is stirred at 60° C. for 15 h before it is diluted with 1 N aq. NaOH (100 mL). The mixture is extracted with diethyl ether (300 mL, 150 mL) and the combined org. extracts are washed with 1 N aq. NaOH (2×100 mL), 1 M aq. NaH2PO4 (50 mL), dried over Na2SO4, filtered and concentrated to give 2-allyloxy-5-bromo-1,3-dimethyl-benzene (23.6 g) as a yellow oil, LC-MS: tR=1.08 min, [M+1]+=241.20.

WORKUP

后处理

  1. extractionThe mixture is extracted with diethyl ether (300 mL, 150 mL)
  2. washextracts are washed with 1 N aq. NaOH (2×100 mL), 1 M aq. NaH2PO4 (50 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated