Reacción #1733646

Ecuación de reacción

2,4-dibromobutyric acid methyl ester

5-amino-2-chloro-4-fluoro-thiophenol

potassium carbonate

→

2-(5-amino-2-chloro-4-fluorophenylthio)-4-bromobutyric acid methyl ester

Disolventes

methyl ethyl ketone

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe reaction mixture is then heated
2. 2
   Temperaturaunder reflux for 2 hours
3. 3
   TemperaturaAfter cooling of the reaction mixture
4. 4
   Filtraciónthe inorganic portion of the mixture is filtered off
5. 5
   Lavadowashed with methyl ethyl ketone
6. 6
   OtroConcentration of the organic solution by evaporation and chromatographic purification of the residue by means of silica gel chromatography yield 25.5 g of 2-(5-amino-2-chloro-4-fluoro-phenylthio)-4-bromobutyric acid methyl ester having a melting point of from +97° to +99° C.

Procedimiento

28.6 g of 2,4-dibromobutyric acid methyl ester are added dropwise at room temperature to a mixture of 17.8 g of 5-amino-2-chloro-4-fluoro-thiophenol and 15.2 g of potassium carbonate in 160 ml of methyl ethyl ketone (exothermic reaction). The reaction mixture is then heated under reflux for 2 hours. After cooling of the reaction mixture, the inorganic portion of the mixture is filtered off and washed with methyl ethyl ketone. Concentration of the organic solution by evaporation and chromatographic purification of the residue by means of silica gel chromatography yield 25.5 g of 2-(5-amino-2-chloro-4-fluoro-phenylthio)-4-bromobutyric acid methyl ester having a melting point of from +97° to +99° C.

Fuente