反应 #979952

反应方程式

4-chloro-2,6-dimethyl-3-nitropyridine

4-aminobenzonitrile

→

4-(4-Cyanophenyl)amino-2,6-dimethyl-3-nitropyridine

溶剂

ethanol

反应条件

后处理

1. 1
   其他The solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane (200 ml)
3. 3
   洗涤washed with saturated aqueous sodium bicarbonate (100 ml)
4. 4
   干燥The organic phase was dried (MgSO4)
5. 5
   浓缩concentrated under reduced pressure
6. 6
   其他to give a gum which
7. 7
   其他was crystallised
8. 8
   workup.ADDITIONby adding ether (100 ml)
9. 9
   其他sonicating for 5 minutes
10. 10
    过滤The yellow solid (9.80 g, 70%) was filtered off
11. 11
    其他dried in vacuo, mp 171°-172° C.

实验过程

A solution of 4-chloro-2,6-dimethyl-3-nitropyridine (9.80 g, 52.5 mmol) and 4-aminobenzonitrile (6.20 g, 52.5 mmol) in ethanol (160 ml) was stirred at room temperature for 16 hours. The solvent was removed under reduced pressure and the residue was dissolved in dichloromethane (200 ml), and washed with saturated aqueous sodium bicarbonate (100 ml). The organic phase was dried (MgSO4) and concentrated under reduced pressure to give a gum which was crystallised by adding ether (100 ml) and sonicating for 5 minutes. The yellow solid (9.80 g, 70%) was filtered off and dried in vacuo, mp 171°-172° C.

来源