HRID1824960

反应详情

EQUATION

反应方程式

HRID 1824960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 0.27 gm (1.15 mMol) ethyl 2-(5-fluorobenzofur-7-yl)propionate in 4 mL dimethylformamide were added sequentially 0.16 mL (3.91 mMol) freshly distilled formamide and 0.81 mL (0.80 mMol) sodium methoxide (1 M in methanol) dropwise and the resulting mixture was heated at 100° C. for 45 minutes. The reaction mixture was cooled to room temperature and was then diluted with 25 volumes of ethyl acetate. The mixture was then washed sequentially with water and saturated aqueous sodium chloride, and concentrated under reduced pressure. The residue was subjected to flash silica gel chromatography, eluting with 2:1 ethyl acetate:hexane. Fractions containing product were combined and concentrated under reduced pressure to provide 0.060 gm (25%) of the desired compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. washThe mixture was then washed sequentially with water and saturated aqueous sodium chloride
  3. concentrationconcentrated under reduced pressure
  4. washeluting with 2:1 ethyl acetate
  5. additionFractions containing product
  6. concentrationconcentrated under reduced pressure