HRID1454111

反应详情

EQUATION

反应方程式

HRID 1454111 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

Under nitrogen atmosphere, a mixture of ethyl (αS)-α-[[(1,1-dimethylethoxy)carbonyl]amino]-4-bromobenzene propanoate (11.17 g), 4-ethoxymethyl-2,6-dimethoxyphenylboronic acid (10.80 g), palladium acetate (0.34 g), triphenylphosphine (1.57 g), anhydrous potassium carbonate (12.44 g), N-methylpyrrolidone (56 ml) and water (11 ml) was stirred for 50 minutes at 80° C. After completion of the reaction, the mixture was cooled to room temperature and extracted with ethyl acetate and water. The organic layer was washed with 10% aqueous citric acid solution and saturated aqueous NaCl solution, dried over magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure to yield ethyl (αS)-α-[[(1,1-dimethylethoxy)carbonyl]amino]-4′-ethoxymethyl-2′,6′-dimethoxy(1,1′-biphenyl)-4-propionate (20.4 g) as oil.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperaturethe mixture was cooled to room temperature
  3. extractionextracted with ethyl acetate and water
  4. washThe organic layer was washed with 10% aqueous citric acid solution and saturated aqueous NaCl solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltrated
  7. concentrationThe filtrate was concentrated under reduced pressure