Reaktion #1857546

ord-b4dc4fa4b836422680bd5a51fce98bcc

Reaktionsgleichung

Cl
hydrochloric acid
c1nc[nH]n1
1,2,4-Triazole
O=C(CBr)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
2-bromo-1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone
[H-].[Na+]
sodium hydride
O=C(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
desired material
Ausbeute 80.3%
O=C(Cn1cncn1)c1ccc(Oc2ccc(Cl)cc2)cc1Cl
1-[2-chloro-4-(4-chlorophenoxy)phenyl]-2-(1,2,4-triazol-1-yl)ethanone
Ausbeute 80.3%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added (3000 mL)
  2. 2
    FiltrationThe precipitate was filtered off
  3. 3
    Waschenwashed with MTBE
  4. 4
    EinengenThe organic phase was then concentrated
  5. 5
    Filtrationthe resulting solid was filtered off

Vorschrift

1,2,4-Triazole (249 g) was added carefully (small portions) to a mixture of sodium hydride (85 g) in THF (6000 mL). After 30 minutes a solution of 2-bromo-1-[2-chloro-4-(4-chlorophenoxy)phenyl]ethanone (1322 g) in THF (500 mL) was slowly added and the mixture was stirred for 150 min. The pH was adjusted to 7 with dil. hydrochloric acid whereupon water was added (3000 mL). The precipitate was filtered off and washed with MTBE. The organic phase was then concentrated and the resulting solid was filtered off to yield the desired material (1008 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09247747B2uspto-grants-2016_02