反应 #1116

ord-c0062b7363ec4154b00b2b22681d2f1d

反应方程式

O=C([O-])O.[Na+]
sodium bicarbonate
CCc1nccc(Cl)c1Cl
3,4-dichloro-2-ethylpyridine
NC1CCC(=Cc2ccc(Cl)cc2Cl)CC1
4-(2,4-dichlorobenzylidene)cyclohexylamine
[Cl-].[NH4+]
ammonium chloride
CCc1nccc(NC2CCC(=Cc3ccc(Cl)cc3Cl)CC2)c1Cl
3-Chloro-4-[4-(2,4-dichlorobenzylidene)cyclohexyl]amino-2-ethylpyridine
收率 7.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling
  2. 2
    萃取extracted with ethyl acetate
  3. 3
    其他The product is purified by chromatography on silica gel

实验过程

1.6 g of 3,4-dichloro-2-ethylpyridine and 2.5 g of 4-(2,4-dichlorobenzylidene)cyclohexylamine are heated at 180° C. for 3.5 hours together with 55 g of ammonium chloride in 9 ml of N-methylpyrrolidone. After cooling, the mixture is poured into saturated sodium bicarbonate solution and extracted with ethyl acetate. The product is purified by chromatography on silica gel using ethyl acetate/heptane 1:4. Yield: 7%

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723450uspto-grants-1998_03