反应 #45575

反应方程式

potassium carbonate

N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide

→

compound

收率 94.0%

4-Amino-6-bromo-5-methoxy-2-methylbiphenyl-3-carbonitrile

收率 94.0%

溶剂

methanol

反应条件

后处理

1. 1
   温度After cooling
2. 2
   其他methanol was evaporated away under reduced pressure
3. 3
   萃取followed by extraction with ethyl acetate
4. 4
   洗涤washing with saturated brine
5. 5
   干燥drying on anhydrous magnesium sulfate
6. 6
   浓缩the solvent was concentrated under reduced pressure
7. 7
   其他to obtain a pale brown residue
8. 8
   其他The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)

实验过程

Aqueous potassium carbonate solution (1.25 ml) [potassium carbonate (15 g) was dissolved in water (100 ml)] and methanol (1.25 ml) were added to N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide (I-38) (133 mg, 0.322 mmol), followed by stirring overnight at 70° C. After cooling, methanol was evaporated away under reduced pressure, followed by extraction with ethyl acetate, washing with saturated brine and drying on anhydrous magnesium sulfate, the solvent was concentrated under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1) to obtain the entitled compound (95 mg, 94%) as a colorless solid.

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