反应 #45580

反应方程式

water

N,N-dimethylformamide

4-bromo-3-fluoro-6-iodo-2-methoxy-5-methylphenylamine

→

compound

收率 80.0%

2-Amino-5-bromo-4-fluoro-3-methoxy-6-methylbenzonitrile

收率 80.0%

溶剂

brine

反应条件

后处理

1. 1
   温度After cooling to room temperature
2. 2
   萃取followed by extraction twice with ethyl acetate
3. 3
   洗涤the organic layer was washed with saturated brine
4. 4
   干燥dried over anhydrous magnesium sulfate
5. 5
   过滤After filtration and concentration under reduced pressure
6. 6
   浓缩the eluate with n-hexane:ethyl acetate (10:1) was concentrated under reduced pressure

实验过程

Under nitrogen atmosphere, water (0.1 ml), zinc cyanide (59 mg, 0.5 mmol), 1,1′-bis(diphenylphosphino)ferrocene (67 mg, 0.12 mmol), bis(dibenzylideneacetone)palladium(0) (58 mg, 0.1 mmol) were added to an N,N-dimethylformamide (10 ml) solution of 4-bromo-3-fluoro-6-iodo-2-methoxy-5-methylphenylamine (I-44) (359 mg, 1.0 mmol), followed by stirring at 120 to 130° C. for 3 hours. After cooling to room temperature, saturated brine was added to the reaction liquid, followed by extraction twice with ethyl acetate, the organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate. After filtration and concentration under reduced pressure, the resulting residue was subjected to column chromatography, and the eluate with n-hexane:ethyl acetate (10:1) was concentrated under reduced pressure to obtain the entitled compound (208 mg, 80%) as a white solid.

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