反应 #554649

ord-f7303ff4a17b4f8ea9c6040a1d9dfb41

反应方程式

N
Ammonia
Clc1ccc(-c2ccc(Cl)nn2)cc1
3-(4-chlorophenyl)-6-chloropyridazine
[I-].[Na+]
NaI
Cl
HCl
Clc1ccc(-c2ccc(I)nn2)cc1
3-(4-chlorophenyl)-6-iodopyridazine

溶剂

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONare added
  2. 2
    萃取extracted with EtOAc
  3. 3
    干燥dried with Na2SO4
  4. 4
    其他the solvent is removed in vacuo
  5. 5
    其他The resulting crude product is triturated with TBME

实验过程

20 ml ACN are added to 0.50 g (1.11 mmol) 3-(4-chlorophenyl)-6-chloropyridazine and 3.33 g (22.2 mmol) NaI before 189 μl fuming conc. HCl are added and the mixture is stirred at 80° C. for 4 h. The mixture is alkalised with aq. Ammonia solution (32%) diluted with water and extracted with EtOAc. The org. phases are combined, dried with Na2SO4 and the solvent is removed in vacuo. The resulting crude product is triturated with TBME.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08623860B2uspto-grants-2014_01