反应 #66517

反应方程式

3-Methoxyaniline

picolinic acid

EDCI.HCl

Et3N

hydroxybenzotriazole

→

N-(3-methoxyphenyl)picolinamide

收率 90.1%

溶剂

DCM

反应条件

后处理

1. 1
   洗涤The organic phase was washed with a saturated solution of NaHCO3 and with brine
2. 2
   干燥was dried over MgSO4
3. 3
   过滤was filtered
4. 4
   浓缩was concentrated under reduced pressure
5. 5
   其他The crude product was purified by flash chromatography over silica gel

实验过程

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.

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