反应 #2487500

反应方程式

chloroacetaldehyde

4-Chloro-pyridin-2-ylamine

NaHCO3

→

product

收率 86.5%

7-Chloro-imidazol[1,2-a]pyridine

收率 86.5%

溶剂

EtOH

反应条件

后处理

1. 1
   温度The mixture was refluxed for 6 h
2. 2
   其他Solvents removed under reduced pressure
3. 3
   其他the crude mixture was partitioned between water and EtOAc
4. 4
   洗涤The organic layer was washed with brine
5. 5
   干燥dried (MgSO4)
6. 6
   过滤filtered
7. 7
   浓缩concentrated under reduced pressure
8. 8
   其他The product was purified by column chromatography (SiO2, eluted with 50% EtOAC-petrol)

实验过程

To a solution of 4-Chloro-pyridin-2-ylamine (12.8 g, 100 mmol, 1.0 equiv) in EtOH (170 ml) was added NaHCO3 (16.8 g, 200 mmol, 2.0 equiv) followed by chloroacetaldehyde (19.0 ml, 150 mmol, 1.5 equiv). The mixture was refluxed for 6 h. Solvents removed under reduced pressure and the crude mixture was partitioned between water and EtOAc. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The product was purified by column chromatography (SiO2, eluted with 50% EtOAC-petrol) to afford 13.2 g of product. MS: [M+H]+=153.

来源