تفاعل #45574

معادلة التفاعل

potassium carbonate

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

→

compound

المردود 91.0%

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

المردود 91.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   أخرىThe reaction liquid
3. 3
   درجة الحرارةwas cooled to room temperature
4. 4
   أخرىmethanol was evaporated away under reduced pressure, water
5. 5
   workup.ADDITIONwas added to the residue
6. 6
   استخلاصfollowed by extraction twice with ethyl acetate
7. 7
   غسيلthe organic layer was washed with saturated brine
8. 8
   تجفيفdried over anhydrous magnesium sulfate
9. 9
   تركيزAfter nitration and concentration under reduced pressure

الإجراء التجريبي

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.

المصدر