Reaktion #45571

Reaktionsgleichung

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

ammonium acetate

→

compound

Ausbeute 50.3%

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

Ausbeute 50.3%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction liquid
2. 2
   Einengenwas concentrated under reduced pressure, ethyl acetate and water
3. 3
   workup.ADDITIONwere added to the residue
4. 4
   Sonstigethe precipitated insoluble matter was separated by filtration
5. 5
   SonstigeThe organic layer was collected by liquid-liquid separation
6. 6
   Waschenwashed with aqueous saturated sodium chloride solution
7. 7
   Trocknendried on anhydrous magnesium sulfate
8. 8
   Sonstigethe solvent was evaporated away under reduced pressure

Vorschrift

Under nitrogen atmosphere, 7-bromo-6-iodo-5-methoxy-5-methyl-1H-benzo[d][1,3]oxazine-2,4-dione (I-32) (3.68 g, 8.93 mmol) and ammonium acetate (3.44 g, 44.7 mmol) were added to dewatered N,N-dimethylformamide (80 ml), followed by stirring at room temperature for 2 hours. The reaction liquid was concentrated under reduced pressure, ethyl acetate and water were added to the residue, the precipitated insoluble matter was separated by filtration. The organic layer was collected by liquid-liquid separation, washed with aqueous saturated sodium chloride solution and dried on anhydrous magnesium sulfate, the solvent was evaporated away under reduced pressure to obtain the entitled compound (1.73 g, 50%) as a brown solid. Not further purified, this was used in the next reaction.

Quelle