Реакция #1857547

ord-a0f60c01467e4bb49e4d352d2ae3b07f

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe mixture was then heated for 10 h
  2. 2
    Температураto reflux
  3. 3
    Другоеthe organic phase was dried
  4. 4
    Другоеevaporated
  5. 5
    Другоеto obtain the crude product
  6. 6
    ДругоеThis was purified by column chromatography

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09247747B2uspto-grants-2016_02