反应 #45571

反应方程式

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

ammonium acetate

→

compound

收率 50.3%

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

收率 50.3%

溶剂

N,N-dimethylformamide

反应条件

后处理

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

实验过程

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.

来源