تفاعل #45571

معادلة التفاعل

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

ammonium acetate

→

compound

المردود 50.3%

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

المردود 50.3%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر