Reacción #45570

Ecuación de reacción

ammonium acetate

7-fluoro-6-iodo-8-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione

→

compound

Rendimiento 96.2%

2-Amino-4-fluoro-5-iodo-3-methoxy-6-methylbenzamide

Rendimiento 96.2%

Disolventes

N,N-dimethylformamide

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe reaction liquid
2. 2
   Concentraciónwas concentrated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
4. 4
   Lavadowashed three times with saturated brine
5. 5
   Secadodried over anhydrous magnesium sulfate
6. 6
   FiltraciónAfter filtration and concentration under reduced pressure
7. 7
   Filtraciónfollowed by filtration
8. 8
   Otrodrying

Procedimiento

Under nitrogen atmosphere, ammonium acetate (4.62 g, 60.0 mmol) was added to an N,N-dimethylformamide (120 ml) solution of 7-fluoro-6-iodo-8-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione (I-31) (4.2 g, 12.0 mmol), followed by stirring at room temperature for 16 hours. The reaction liquid was concentrated under reduced pressure, the residue was dissolved in ethyl acetate, washed three times with saturated brine, then dried over anhydrous magnesium sulfate. After filtration and concentration under reduced pressure, the resulting residue was suspended in diisopropyl ether, followed by filtration and drying to obtain the entitled compound (3.74 g, 96%) as a white solid.

Fuente