Reaktion #792140

ord-d141f4d160b54c5593da59aedd2a5554

Reaktionsgleichung

[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

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture extracted with MTBE
  2. 2
    Waschenwashed with an aqueous solution of lithium chloride
  3. 3
    SonstigeThe crude residue was purified by recrystallization in diisopropylether

Vorschrift

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.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09173402B2uspto-grants-2015_11