HRID1675580

反应详情

EQUATION

反应方程式

HRID 1675580 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a mixture obtained by adding 5.0 g of 2-propynyl 3,4,5-trifluorobenzoate and 1.7 g of propargyl alcohol to 20 ml of DMF was added 1.1 g of 60% sodium hydride (oily) at 0° C. The resulting mixture was stirred at 0° C. for 30 minutes, and then at room temperature for 1 hour. Thereafter, water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and 2.9 g of 2-propynyl 3,5-difluoro-4-(2-propynyloxy)benzoate was obtained.

WORKUP

后处理

  1. customTo a mixture obtained
  2. waitat room temperature for 1 hour
  3. extractionfollowed by extraction with ethyl acetate
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure