反应 #554650

ord-c3404dcd9c87462eb1a1f76a790d43c0

反应方程式

[Na]
sodium
CCCO
n-propanol
Clc1cc(I)ccn1
2-chloro-4-iodo-pyridine
CCCOc1cc(I)ccn1
4-Iodo-2-propoxy-pyridine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISSOLUTIONis dissolved completely (ca. 45 min)
  2. 2
    workup.STIRRINGThe mixture is stirred
  3. 3
    温度at reflux for 3 h
  4. 4
    其他The reaction is quenched by the addition of some water
  5. 5
    其他The solvent is removed in vacuo and to the residue
  6. 6
    workup.ADDITIONare added 20 mL DMF/MeOH
  7. 7
    过滤The mixture is filtrated
  8. 8
    其他the filtrate is purified by HPLC (MeOH/H2O/NH3)

实验过程

0.58 g (25.06 mmol) sodium are carefully added to 40 mL n-propanol by several portions. The mixture is stirred until the metal is dissolved completely (ca. 45 min). Then 6.00 g (25.1 mmol) 2-chloro-4-iodo-pyridine are slowly added to the mixture. The mixture is stirred at reflux for 3 h. The reaction is quenched by the addition of some water. The solvent is removed in vacuo and to the residue are added 20 mL DMF/MeOH. The mixture is filtrated and the filtrate is purified by HPLC (MeOH/H2O/NH3).

来源

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