Réaction #76774

Équation de réaction

sodium acetate

1,1-dibromo-3,3,3-trifluoroacetone

ethyl 2-chloro-5-hydrazinocinnamate

→

ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate

Rendement 97.5%

Solvants

water

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source