反応 #1106

ord-ed5d30e63cae482aa9ed8a44a63361f9

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling
  2. 2
    抽出the product is extracted
  3. 3
    濃縮After concentrating
  4. 4
    workup.DISTILLATIONthe excess of amine is distilled off in vacuo
  5. 5
    その他the residue is crystallized

実験手順

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%

出典

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