反応 #45571

反応方程式

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

ammonium acetate

→

compound

収率 50.3%

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

収率 50.3%

溶媒

N,N-dimethylformamide

反応条件

後処理

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

実験手順

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.

出典