تفاعل #76774

ord-f6842c74bf1f4c02a4882ecb818c07ca

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added at 10° C.
  2. 2
    workup.STIRRINGlower, and the mixture was stirred for 3 hours
  3. 3
    ترشيحThe precipitated crystals were collected by filtration
  4. 4
    أخرىdried

الإجراء التجريبي

First, 7.4 g (90.2 mmol) of sodium acetate and 8.0 g (28.2 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone were mixed with 70 ml of water, and the mixture was stirred at 80° C. for 30 minutes and then cooled, to which 7.0 g of ethyl 2-chloro-5-hydrazinocinnamate was added at 10° C. or lower, and the mixture was stirred for 3 hours. The precipitated crystals were collected by filtration and dried, which afforded 9.6 g (27.5 mmol) of ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06703503B2uspto-grants-2004_03