HRID2247440

反应详情

EQUATION

反应方程式

HRID 2247440 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

357 mg of Methyl (4′-methoxy-3′-trifluoromethanesulfonyloxybiphenyl-3-yl)acetate was dissolved in 3 ml of N,N-dimethylformamide, then 0.45 ml of butyl vinyl ether, 10 mg of palladium acetate, 20 mg of diphenyl phosphinopropane and 1 ml of triethylamine were added thereto, and the mixture was stirred at 80° C. overnight in a nitrogen atmosphere. The reaction mixture was diluted with ethyl acetate and washed with 1N hydrochloric acid. The organic layer was dried over anhydrous magnesium sulfate and then filtered, and the filtrate was concentrated. The residue was purified by silica gel column chromatography, to give 184 mg of the title compound in the 4:1 hexane-ethyl acetate fraction.

WORKUP

后处理

  1. washwashed with 1N hydrochloric acid
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by silica gel column chromatography