Reacción #2045093
ord-457ecc6eabfb4774b861b707817d9960
Ecuación de reacción
2-bromo-1-(4-chlorophenyl)ethanone
acetonitrile
→
2-amino-1-(4-chlorophenyl)ethanone hydrochloride
Rendimiento 50.0%
Reactivos
Ninguno
Condiciones de reacción
Temperatura
105°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Temperaturawas heated
- 2OtroThe formed sodium bromide was removed by filtration
- 3Concentraciónthe filtrate concentrated in vacuo
- 4workup.DISSOLUTIONThe residue was dissolved in ethanol (2.5 mL per mmol)
- 5workup.ADDITIONconc. aq. hydrochloric acid (0.9 mL per mmol) added at ambient temperature
- 6Filtraciónwere filtered off
- 7Lavadowashed with ethanol (1×0.5 mL per mmol)
- 8OtroDrying of the solids
Procedimiento
A mixture of 2-bromo-1-(4-chlorophenyl)ethanone (1.0 eq.) and NaN(CHO)2 (1.1 eq.) in acetonitrile (1.5 mL per mmol) was heated to reflux for 4 h at 105° C. ext. temperature. The formed sodium bromide was removed by filtration and the filtrate concentrated in vacuo. The residue was dissolved in ethanol (2.5 mL per mmol) and conc. aq. hydrochloric acid (0.9 mL per mmol) added at ambient temperature. After stirring for 72 h at room temperature the solids were filtered off and washed with ethanol (1×0.5 mL per mmol). Drying of the solids afforded 2-amino-1-(4-chlorophenyl)ethanone hydrochloride in ca. 50% yield that was used in the next step without purification.