تفاعل #45575

معادلة التفاعل

potassium carbonate

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

→

compound

المردود 94.0%

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

المردود 94.0%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   أخرىmethanol was evaporated away under reduced pressure
3. 3
   استخلاصfollowed by extraction with ethyl acetate
4. 4
   غسيلwashing with saturated brine
5. 5
   تجفيفdrying on anhydrous magnesium sulfate
6. 6
   تركيزthe solvent was concentrated under reduced pressure
7. 7
   أخرىto obtain a pale brown residue
8. 8
   أخرىThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)

الإجراء التجريبي

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.

المصدر