反应 #2507843

反应方程式

Hydrochloric acid

2-propynyl 2-chloro-4,5-difluorobenzoate

propargyl alcohol

sodium hydride

→

2-propynyl 2-chloro-5-fluoro-4-(2-propynyloxy)benzoate

收率 129.4%

溶剂

DMF

反应条件

后处理

1. 1
   温度cooling
2. 2
   萃取followed by extraction with ethyl acetate
3. 3
   洗涤The resulting organic layer was washed sequentially with water
4. 4
   干燥an aqueous saturated sodium chloride solution, dried over magnesium sulfate
5. 5
   浓缩concentrated under reduced pressure

实验过程

To a mixture of 150 ml of DMF, 12.7 g of 2-propynyl 2-chloro-4,5-difluorobenzoate and 3.4 g of propargyl alcohol was added 2.4 g of 60% sodium hydride (oily) under ice-cooling. The reaction mixture was stirred at room temperature overnight. Hydrochloric acid was added to the reaction mixture, followed by extraction with ethyl acetate. The resulting organic layer was washed sequentially with water and an aqueous saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography, and 19 g of 2-propynyl 2-chloro-5-fluoro-4-(2-propynyloxy)benzoate was obtained.

来源