반응 #45570

반응 방정식

ammonium acetate

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

→

compound

수율 96.2%

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

수율 96.2%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The reaction liquid
2. 2
   농축was concentrated under reduced pressure
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
4. 4
   세척washed three times with saturated brine
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   여과After filtration and concentration under reduced pressure
7. 7
   여과followed by filtration
8. 8
   기타drying

실험 절차

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.

출처