反应 #2320162

反应方程式

pyridin-3-ol

NaH

2-chloronicotinonitrile

→

product

收率 55.8%

2-(Pyridin-3-yloxy)-nicotinonitrile

收率 55.8%

溶剂

N,N-dimethyl formamide

反应条件

后处理

1. 1
   其他The reaction mixture was quenched with 1M NaHCO3
2. 2
   萃取extracted with ethyl acetate (3×30 ml)
3. 3
   洗涤The combined organic extracts were washed with saturated NaCl (50 ml)
4. 4
   干燥dried (Na2SO4)
5. 5
   过滤filtered
6. 6
   浓缩concentrated
7. 7
   其他The crude product was purified by flash column chromatography

实验过程

To a solution of pyridin-3-ol (1.3 g, 10 mmol) in N,N-dimethyl formamide (25 ml) was added 60 % NaH in mineral oil (0.3 g, 15 mmol) and 2-chloronicotinonitrile (1.38 g, 10 mmol) and heated at 120° C. for overnight. The reaction mixture was quenched with 1M NaHCO3 and extracted with ethyl acetate (3×30 ml). The combined organic extracts were washed with saturated NaCl (50 ml), dried (Na2SO4), filtered and concentrated. The crude product was purified by flash column chromatography using dichloromethane to yield 1.1 g (50%) of product. MS (ESI+) m/z 198 (M+H)+.

来源