HRID1261521

反应详情

EQUATION

反应方程式

HRID 1261521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

850 mg (1.9 mmol) of ethyl 3″-tert-butyl-4″-diethylamino-4′-hydroxy[1,1′;3′,1″]terphenyl-4-carboxylate (obtained in Example 1d) are dissolved in dimethylformamide under nitrogen. 92 mg (2.3 mmol) of 60% sodium hydride are added. After 20 minutes at room temperature, 0.25 mL (2.3 mmol) of 2-bromoethan-1-ol acetate are added and the mixture is stirred for 24 hours at room temperature and then poured into saturated ammonium chloride solution and extracted with ethyl acetate. The organic phase is washed with water and then dried and evaporated. The residue obtained is purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate). 1 g of ethyl 4′-(2-acetoxyethoxy)-3″-tert-butyl-4″-diethylamino[1,1′;3′,1″]terphenyl-4-carboxylate is obtained (yield=99%) in the form of a colorless oil.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe organic phase is washed with water
  3. customdried
  4. customevaporated
  5. customThe residue obtained
  6. customis purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate)