Reacción #44400
ord-258c082de91b464ba0230efdebd317cf
Ecuación de reacción
hydrochloride
trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride
triethylamine
triphosgene
triethylamine
→
title compound
Rendimiento 143.6%
Trans-1-{4-[2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl]-cyclohexyl}-3,3-dimethyl-urea
Rendimiento 143.6%
Reactantes
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1workup.ADDITIONwas dropped in
- 2workup.ADDITIONwas added
- 3FiltraciónThe mixture was filtered
- 4Lavadothe filtrate washed with water
- 5Otrodried
- 6Otroevaporated in vacuo
- 7OtroRecrystallizing the product from methanol
Procedimiento
0.56 g (1.2 mmol) trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride was suspended in dry dichloromethane (50 ml), triethylamine 0.77 ml, 6 mmol) was added and 0.13 g (0.44 mmol) triphosgene dissolved in dichloromethane was dropped in. After one hour stirring at room temperature dimetilamine hydrochloride (0.49 g, 6 mmol) followed by triethylamine (0.84 ml, 6 mmol) was added and the stirring was continued for 20 hours. The mixture was filtered, the filtrate washed with water, dried and evaporated in vacuo. Recrystallizing the product from methanol gave the title compound (0.27 g, 52%). Melting point: 212-4° C.