反应详情

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.

1. temperatureThe reaction mixture is then heated
2. temperatureunder reflux for 18 hours
3. temperatureAfter cooling of the reaction mixture
4. filtrationthe inorganic portion of the mixture is filtered off
5. washwashed with methyl ethyl ketone
6. customConcentration 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.