Реакция #1857546

ord-b4dc4fa4b836422680bd5a51fce98bcc

Уравнение реакции

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
Выход 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
Выход 80.3%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.ADDITIONwas added (3000 mL)
  2. 2
    ФильтрацияThe precipitate was filtered off
  3. 3
    Промывкаwashed with MTBE
  4. 4
    КонцентрированиеThe organic phase was then concentrated
  5. 5
    Фильтрацияthe resulting solid was filtered off

Методика

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).

Источник

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