反应 #336436

反应方程式

3-amino-4-[N-(4-cyanophenyl)amino]pyridine

3-Amino-4-[N-(4-cyanophenyl)amino]pyridine

triethyl orthoacetate

→

title compound

1-(4-Cyanophenyl)-2-methylimidazo[4,5-c]pyridine

溶剂

acetic anhydride

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度under reflux for 2 hours under nitrogen
3. 3
   温度cooled
4. 4
   浓缩concentrated under reduced pressure The brown residue
5. 5
   workup.DISSOLUTIONwas dissolved in 1M hydrochloric acid
6. 6
   洗涤washed with ethyl acetate (200 ml)
7. 7
   萃取extracted with dichloromethane (3×200 ml)
8. 8
   洗涤The combined extracts were washed with water
9. 9
   干燥dried (MgSO4)
10. 10
    浓缩concentrated

实验过程

A mixture of 3-amino-4-[N-(4-cyanophenyl)amino]pyridine (see part (b)) (9.31 g, 44.3 mmol), triethyl orthoacetate (40 ml) and acetic anhydride (30 ml) was heated under reflux for 2 hours under nitrogen, cooled, then concentrated under reduced pressure The brown residue was dissolved in 1M hydrochloric acid and washed with ethyl acetate (200 ml). The aqueous layer was rendered basic with saturated aqueous ammonia and extracted with dichloromethane (3×200 ml). The combined extracts were washed with water, dried (MgSO4) and concentrated to give the title compound (6.5 g), as a brown solid.

来源