تفاعل #44400

معادلة التفاعل

hydrochloride

trans-4-{2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl}-cyclohexyl-amine trihydrochloride

triethylamine

triphosgene

triethylamine

→

title compound

المردود 143.6%

Trans-1-{4-[2-[4-(2,3-dichlorophenyl)-piperazin-1-yl]-ethyl]-cyclohexyl}-3,3-dimethyl-urea

المردود 143.6%

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas dropped in
2. 2
   workup.ADDITIONwas added
3. 3
   ترشيحThe mixture was filtered
4. 4
   غسيلthe filtrate washed with water
5. 5
   أخرىdried
6. 6
   أخرىevaporated in vacuo
7. 7
   أخرىRecrystallizing the product from methanol

الإجراء التجريبي

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.

المصدر