反応 #1857547

ord-a0f60c01467e4bb49e4d352d2ae3b07f

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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