反应 #1106

ord-ed5d30e63cae482aa9ed8a44a63361f9

反应方程式

COc1c(Cl)ccnc1C
4-chloro-3-methoxy-2-methylpyridine
CC(C)(C)c1ccc(N)cc1
4-tert-butylaniline
[Na+].[OH-]
NaOH
COc1c(Nc2ccc(C(C)(C)C)cc2)ccnc1C
4-(4-tert-Butylanilino)-3-methoxy-2-methylpyridine

溶剂

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the product is extracted
  3. 3
    浓缩After concentrating
  4. 4
    workup.DISTILLATIONthe excess of amine is distilled off in vacuo
  5. 5
    其他the residue is crystallized

实验过程

7.9 g of 4-chloro-3-methoxy-2-methylpyridine and 22.4 g of 4-tert-butylaniline are heated at 120° C. for 8 hours in 20 g of phenol. After cooling, the mixture is poured into NaOH and the product is extracted using methylene chloride. After concentrating, the excess of amine is distilled off in vacuo and the residue is crystallized using hexane. 9.5 g=55%

来源

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