HRID253484

反应详情

EQUATION

反应方程式

HRID 253484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

320 μl (3.14 mmol) of 1,3-dibromopropane and 440 mg (3.18 mmol) of potassium carbonate are added to a solution of 900 mg (2.1 mmol, 1 eq) of ethyl 4′-hydroxy-3′-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphth-2-yl)biphenyl-4-carboxylate in 30 ml of methyl ethyl ketone. The reaction mixture is stirred overnight at room temperature and then for 1 day at reflux. The medium is cooled to room temperature and then filtered. The filtrate is evaporated and the residue is purified by chromatography on silica gel (eluent: 90/10 heptane/ethyl acetate). 640 mg of ethyl 4′-(3-bromopropoxy)-3′-(5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphth-2-yl)biphenyl-4-carboxylate are obtained in the form of a white solid (yield=55%).

WORKUP

后处理

  1. temperaturefor 1 day at reflux
  2. temperatureThe medium is cooled to room temperature
  3. filtrationfiltered
  4. customThe filtrate is evaporated
  5. customthe residue is purified by chromatography on silica gel (eluent: 90/10 heptane/ethyl acetate)