Реакция #45571

Уравнение реакции

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

ammonium acetate

→

compound

Выход 50.3%

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

Выход 50.3%

Растворители

N,N-dimethylformamide

Условия реакции

Обработка

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

Методика

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.

Источник