反应 #45574

反应方程式

potassium carbonate

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

→

compound

收率 91.0%

4-Amino-3-cyano-6-fluoro-5-methoxy-2-methylbiphenyl

收率 91.0%

溶剂

methanol

反应条件

后处理

1. 1
   其他The reaction liquid
2. 2
   其他The reaction liquid
3. 3
   温度was cooled to room temperature
4. 4
   其他methanol was evaporated away under reduced pressure, water
5. 5
   workup.ADDITIONwas added to the residue
6. 6
   萃取followed by extraction twice with ethyl acetate
7. 7
   洗涤the organic layer was washed with saturated brine
8. 8
   干燥dried over anhydrous magnesium sulfate
9. 9
   浓缩After nitration and concentration under reduced pressure

实验过程

Aqueous 20% (w/v) potassium carbonate solution (9.0 ml, 13.0 mmol) was added to a methanol (9 ml) suspension of N-(5-cyano-2-fluoro-3-methoxy-6-methylbiphenyl-4-yl)-2,2,2-trifluoroacetamide (I-37) (400 mg, 1.14 mmol), followed by stirring at 70° C. for 16 hours. The reaction liquid became uniform with temperature elevation. The reaction liquid was cooled to room temperature, methanol was evaporated away under reduced pressure, water was added to the residue, followed by extraction twice with ethyl acetate, the organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate. After nitration and concentration under reduced pressure, the entitled compound (266 mg, 91%) was obtained as a white solid.

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