HRID1158149

反应详情

EQUATION

反应方程式

HRID 1158149 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1 g of ethyl 3″-tert-butyl-4″-diethylamino-4′-hydroxy[1,1′;3′,1″]terphenyl-4-carboxylate obtained in Example 1d (2.2 mmol) are dissolved in 20 mL of dimethylformamide under a nitrogen atmosphere. 880 mg (2.7 mmol) of caesium carbonate are added. The reaction medium stirred at room temperature turns yellow. 0.64 mL of 1-bromo-4-(tert-butyldimethylsilanyloxy)butane (2.4 mmol) is then added and the reaction medium is heated at 80° C. for 18 hours. The reaction medium is then cooled to room temperature and then filtered. The solvents are evaporated off and the residue obtained is purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate).

WORKUP

后处理

  1. temperaturethe reaction medium is heated at 80° C. for 18 hours
  2. temperatureThe reaction medium is then cooled to room temperature
  3. filtrationfiltered
  4. customThe solvents are evaporated off
  5. customthe residue obtained
  6. customis purified by chromatography on silica gel (eluent: 70/30 heptane/ethyl acetate)