HRID1422596

反应详情

EQUATION

反应方程式

HRID 1422596 的结构方程式

CONDITIONS

反应条件

温度
11.5 °C

PROCEDURE

实验过程

To a solution of allyl alcohol (48.3 g, 56.5 ml, 831 mmol, Eq: 10) and triethylamine (12.6 g, 17.4 ml, 125 mmol, Eq: 1.5) at 0° C. was added 2-(3-nitrophenyl)acetyl chloride (intermediate B2a) (16.59 g, 83.1 mmol, Eq: 1.00) and the mixture was stirred at 0 to 23° C. for 2 h. Poured into water, extracted with ethyl acetate, washed organic layer with brine and dried over Na2SO4. Removal of the solvent in vacuum left a light brown oil, which was purified by silica gel flash chromatography with n-heptane/ethyl acetate to give the title compounds as a yellow liquid (14.89 g, 81%).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washwashed organic layer with brine
  3. dry with materialdried over Na2SO4
  4. customRemoval of the solvent in vacuum
  5. waitleft a light brown oil, which
  6. customwas purified by silica gel flash chromatography with n-heptane/ethyl acetate