HRID1893071

反应详情

EQUATION

反应方程式

HRID 1893071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

180 mL of N,N-dimethylacetamide (DMA) solution including 12.8 g (60.1 mmol) of potassium phosphate, 14.3 g (48 mmol) of 4-(4-bromophenyl)cyclohexanecarboxylic acid methyl ester produced in Example 1-1, and 8.33 g (40 mmol) of 1-pentyl-4-vinyl-cyclohexane was poured to flask filled with Argon gas. Then, 0.17 g (catalytic amount) of palladium acetate was added to the flask and reacted in oil bath at 120° C. for 32 hours. After reaction, 100 mL of distilled water was added to the reaction mixture, extracted by ethyl acetate, and then the aqueous layer was extracted by chloroform. The organic layer was dried by Na2SO4, concentrated under reduced pressure, and then recrystallized from ethanol to obtain 9.8 g (62%) of 4-{4-[2-(4-pentyl-cyclohexyl)-ethenyl]-phenyl}cyclohexane carboxylic acid methyl ester.

WORKUP

后处理

  1. additionwas poured to flask
  2. additionfilled with Argon gas
  3. customreacted in oil bath at 120° C. for 32 hours
  4. additionwas added to the reaction mixture
  5. extractionextracted by ethyl acetate
  6. extractionthe aqueous layer was extracted by chloroform
  7. dry with materialThe organic layer was dried by Na2SO4
  8. concentrationconcentrated under reduced pressure
  9. customrecrystallized from ethanol