Reacción #1733639

Ecuación de reacción

2,4-dichlorobutyric acid ethyl ester

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

potassium carbonate

→

2-(5-amino-2-chloro-4-fluoro-phenylthio)-4-chlorobutyric acid ethyl ester

Disolventes

methyl ethyl ketone

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe reaction mixture is then heated
2. 2
   Temperaturaunder reflux for 18 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 silica gel chromatography yield 14.2 g of 2-(5-amino-2-chloro-4-fluorophenylthio)-4-chlorobutyric acid ethyl ester having a melting point of from +97° to +99° C.

Procedimiento

At room temperature, 16.2 g of 2,4-dichlorobutyric acid ethyl ester are added dropwise to a mixture of 14 g of 5-amino-2-chloro-4-fluoro-thiophenol and 12.7 g of potassium carbonate in 280 ml of methyl ethyl ketone (exothermic reaction). The reaction mixture is then heated under reflux for 18 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 silica gel chromatography yield 14.2 g of 2-(5-amino-2-chloro-4-fluorophenylthio)-4-chlorobutyric acid ethyl ester having a melting point of from +97° to +99° C.

Fuente