Reacción #41697

Ecuación de reacción

ammonium chloride

2-fluoro-N-methoxy-N-methylbenzamide

→

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

Disolventes

methanol

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Otrothe reaction liquid
2. 2
   Temperaturawas heated
3. 3
   Temperaturaunder reflux for 3 hours
4. 4
   OtroThe reaction liquid
5. 5
   Filtraciónwas filtered through Celite
6. 6
   Otrothe solvent was evaporated away under reduced pressure
7. 7
   workup.ADDITIONThe resulting residue was diluted with ethyl acetate
8. 8
   Lavadowashed with water
9. 9
   Secadodried with anhydrous magnesium sulfate
10. 10
    OtroThe solvent was evaporated away under reduced pressure
11. 11
    Otrothe resulting residue was purified through silica gel column chromatography (
12. 12
    Otrohexane/ethyl acetate=9/1 to 1/2 to obtain the entitled compound as a brown oily substance

Procedimiento

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.

Fuente