Реакция #792140

ord-d141f4d160b54c5593da59aedd2a5554

Уравнение реакции

[Na+].[OH-]
sodium hydroxide
c1c[nH]nn1
triazole
CCC1(c2ccc(Oc3ccc(Cl)cc3)cc2Cl)CO1
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-ethyl-oxirane
CN1CCCC1=O
N-methyl-2-pyrrolidon
[Cl-].[NH4+]
ammonium chloride
CCC(O)(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)butan-2-ol

Условия реакции

Температура
140°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияthe mixture extracted with MTBE
  2. 2
    Промывкаwashed with an aqueous solution of lithium chloride
  3. 3
    ДругоеThe crude residue was purified by recrystallization in diisopropylether

Методика

To 2-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-ethyl-oxirane (216.0 g, 0.63 mol) dissolved in N-methyl-2-pyrrolidon (2 L) was added sodium hydroxide (62.87 g, 1.57 mol) and triazole (217.1 g, 3.14 mol) at room temperature. The mixture was then stirred for 12 hours at 140° C. A solution of ammonium chloride and ice water was then added, the mixture extracted with MTBE and washed with an aqueous solution of lithium chloride. The crude residue was purified by recrystallization in diisopropylether to give 2-[2-chloro-4-(4-chlorophenoxy)phenyl]-1-(1,2,4-triazol-1-yl)butan-2-ol compound as a colorless solid (127.0 g, 51%; m.p.=140-142° C.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09173402B2uspto-grants-2015_11