تفاعل #1857546

ord-b4dc4fa4b836422680bd5a51fce98bcc

معادلة التفاعل

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
المردود 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
المردود 80.3%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added (3000 mL)
  2. 2
    ترشيحThe precipitate was filtered off
  3. 3
    غسيلwashed with MTBE
  4. 4
    تركيزThe organic phase was then concentrated
  5. 5
    ترشيحthe resulting solid was filtered off

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09247747B2uspto-grants-2016_02