تفاعل #45599

معادلة التفاعل

N,N-dimethylformamide

N-(2-cyano-5-fluoro-4-iodo-6-methoxy-3-methylphenyl)-2,2-dimethylpropionamide

phenylboronic acid

→

compound

المردود 96.0%

N-(5-Cyano-2-fluoro-3-methoxy-6-methylbiphenyl-4-yl)-2,2-dimethylpropionamide

المردود 96.0%

المذيبات

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction liquid
2. 2
   درجة الحرارةwas cooled
3. 3
   غسيلby washing with saturated brine (50 ml×3)
4. 4
   تجفيفdrying over anhydrous magnesium sulfate, concentration under reduced pressure
5. 5
   أخرىThe residue was purified twice by silica gel column chromatography (chloroform), (n-hexane:ethyl acetate=4:1)

الإجراء التجريبي

Tetrakis(triphenylphosphine)palladium(0) (1.45 g, 1.26 mmol) was added to an N,N-dimethylformamide (50 ml) suspension of N-(2-cyano-5-fluoro-4-iodo-6-methoxy-3-methylphenyl)-2,2-dimethylpropionamide (I-69) (2.45 g, 6.28 mmol), phenylboronic acid (1.15 g, 9.42 mmol), potassium phosphate n-hydrate (74-78%, 3.60 g, 12.6 mmol), followed by stirring at 95° C. for 2 hours. The reaction liquid was cooled, then ethyl acetate (200 ml) was added, followed by washing with saturated brine (50 ml×3), drying over anhydrous magnesium sulfate, concentration under reduced pressure. The residue was purified twice by silica gel column chromatography (chloroform), (n-hexane:ethyl acetate=4:1) to obtain the entitled compound (2.06 g, 96%) as a yellow solid.

المصدر