تفاعل #66517

معادلة التفاعل

3-Methoxyaniline

picolinic acid

EDCI.HCl

Et3N

hydroxybenzotriazole

→

N-(3-methoxyphenyl)picolinamide

المردود 90.1%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   غسيلThe organic phase was washed with a saturated solution of NaHCO3 and with brine
2. 2
   تجفيفwas dried over MgSO4
3. 3
   ترشيحwas filtered
4. 4
   تركيزwas concentrated under reduced pressure
5. 5
   أخرىThe crude product was purified by flash chromatography over silica gel

الإجراء التجريبي

According to Scheme 1 Method B: 3-Methoxyaniline (1.62 mmol, 0.18 mL) was added to a solution of picolinic acid (1.62 mmol, 0.20 g), EDCI.HCl (2.44 mmol, 0.47 g), Et3N (3.25 mmol, 0.45 mL), hydroxybenzotriazole (1.95 mmol, 0.30 g) in DCM (6 mL) at room temperature. The reaction mixture was stirred at 50° C. for 12 hours. The organic phase was washed with a saturated solution of NaHCO3 and with brine, was dried over MgSO4, was filtered and was concentrated under reduced pressure. The crude product was purified by flash chromatography over silica gel using cyclohexane/AcOEt (90:10) as eluent to afford N-(3-methoxyphenyl)picolinamide (1.46 mmol, 0.33 g, 90%) as an orange liquid.

المصدر