反应 #41697

反应方程式

ammonium chloride

2-fluoro-N-methoxy-N-methylbenzamide

→

4-amino-2-fluoro-N-methoxy-N-methylbenzamide

溶剂

methanol

water

反应条件

后处理

1. 1
   其他the reaction liquid
2. 2
   温度was heated
3. 3
   温度under reflux for 3 hours
4. 4
   其他The reaction liquid
5. 5
   过滤was filtered through Celite
6. 6
   其他the solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe resulting residue was diluted with ethyl acetate
8. 8
   洗涤washed with water
9. 9
   干燥dried with anhydrous magnesium sulfate
10. 10
    其他The solvent was evaporated away under reduced pressure
11. 11
    其他the resulting residue was purified through silica gel column chromatography (
12. 12
    其他hexane/ethyl acetate=9/1 to 1/2 to obtain the entitled compound as a brown oily substance

实验过程

15.2 g of ammonium chloride and 8 g of iron powder were added to a suspension of 10.84 g of 2-fluoro-N-methoxy-N-methylbenzamide in 60 ml of methanol and 30 ml of water, and the reaction liquid was heated under reflux for 3 hours. The reaction liquid was filtered through Celite, and the solvent was evaporated away under reduced pressure. The resulting residue was diluted with ethyl acetate, washed with water, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=9/1 to 1/2 to obtain the entitled compound as a brown oily substance.

来源