HRID1937749

反应详情

EQUATION

反应方程式

HRID 1937749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension obtained by dispersing an about 93:7 mixture (22.1 g) of 2,4-bis(hydroxymethyl)bromobenzene and 2,6-bis(hydroxymethyl)bromobenzene, and p-toluenesulfonic acid monohydrate (0.1 g) in toluene (220 ml) was added dropwise ethyl vinyl ether (18.4 g) at 24-32° C., and the mixture was stirred at room temperature for 2 hr. The reaction mixture was poured into 5% aqueous sodium carbonate solution (100 ml), and the organic layer was washed with 5% aqueous sodium carbonate solution (100 ml), and dried over potassium carbonate. The solvent was evaporated to give an about 93:7 mixture (35.7 g, 97.1%) of 2,4-bis(1′-ethoxyethoxymethyl)bromobenzene and 2,6-bis(1′-ethoxyethoxymethyl)bromobenzene as a yellow oil. 2,4-bis(1′-Ethoxyethoxymethyl)bromobenzene was isolated by preparative HPLC and used in the measurement.

WORKUP

后处理

  1. customTo a suspension obtained
  2. washthe organic layer was washed with 5% aqueous sodium carbonate solution (100 ml)
  3. dry with materialdried over potassium carbonate
  4. customThe solvent was evaporated