HRID2164733

反应详情

EQUATION

反应方程式

HRID 2164733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

20.3 g of succinic acid methyl ester chloride and then a solution of 27 g of 1-(4-phenylbutyl)-imidazole in 100 ml of 1,2-dichloroethane are added dropwise to a suspension of 59.3 g of aluminium chloride in 200 ml of 1,2-dichloroethane, whilst cooling with ice. The mixture is then stirred at 85° C. for 3 hours. After it has been cooled, the reaction mixture is stirred into a mixture of 165.7 g of ethylenediaminetetraacetic acid and 600 g of ice and is brought to about pH 8 by addition of dilute sodium hydroxide solution. The phases are separated and the organic phase is dried over Na2SO4 and concentrated. The residue is purified by column chromatography (silica gel/chloroform).

WORKUP

后处理

  1. temperaturewhilst cooling with ice
  2. temperatureAfter it has been cooled
  3. customThe phases are separated
  4. dry with materialthe organic phase is dried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue is purified by column chromatography (silica gel/chloroform)