反应详情

A mixture of N-(3-cyanophenyl)-N′-((N-benzyl)piperidin-3-yl)cycloheptyl-urea (prepared in Example 60, 2.7 g, 6.98 mmol) and α-chloroethyl chloroformate (1.09 g, 7.65 mmol) was stirred at ambient temperature for 2.5 h, whereupon the reaction was complete as judged by TLC. The solvent was removed by evaporation in vaccuo and was replaced with methanol (40 mL). The reaction was heated at reflux until all of the newly formed intermediate was consumed as indicated by TLC. Evaporation of the solvent gave 2.49 g of N-(3-cyanophenyl)-N′-(piperidin-3-yl)cycloheptylurea; LRMS (M+H)+ m/z 299.

1. customThe solvent was removed by evaporation in vaccuo
2. temperatureThe reaction was heated
3. temperatureat reflux until all of the newly formed intermediate
4. customwas consumed
5. customEvaporation of the solvent