反应 #1857547

ord-a0f60c01467e4bb49e4d352d2ae3b07f

反应方程式

ClCCl
dichloro methane
[H-].[Na+]
sodium hydride
C=CC(O)(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)but-3-en-2-ol
CI
methyl iodide
C=CC(Cn1cncn1)(OC)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
desired compound
C=CC(Cn1cncn1)(OC)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-methoxy-but-3-enyl]-1,2,4-triazole

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was then heated for 10 h
  2. 2
    温度to reflux
  3. 3
    其他the organic phase was dried
  4. 4
    其他evaporated
  5. 5
    其他to obtain the crude product
  6. 6
    其他This was purified by column chromatography

实验过程

2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)but-3-en-2-ol (0.4 g) was dissolved in THF (10 mL) and sodium hydride (0.03 g) was added. The mixture was stirred for 30 min at room temperature and methyl iodide (0.08 mL) was added. The mixture was then heated for 10 h to reflux. Brine and dichloro methane were added, the organic phase was dried and evaporated to obtain the crude product. This was purified by column chromatography to obtain 0.04 g of the desired compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09247747B2uspto-grants-2016_02