反应详情

温度

24 °C

A solution of l-benzyl-4-[1-(t-butoxycarbonyl)-4-piperidylcarbonyl]piperazine (115.7 g) in dry dichloromethane (222 ml) was added dropwise over 45 minutes to trifluoroacetic acid (575 ml), maintaining the temperature below 25° C. under an atmosphere of argon. The solution was stirred at 23-25° C. for 1 hour. The solution was evaporated using a bath temperature of 30° C. The residual oil was poured, in portions, into saturated aqueous sodium carbonate solution (770 ml) while maintaining the temperature below 30° C. The aqueous mixture was extracted with dichloromethane (3×575 ml). The dichloromethane extracts were combined, dried (Na2SO4) and evaporated to give 1-benzyl-4-(4-piperidylcarbonyl)piperazine (56.2 g, 65% yield) as a colourless solid;

1. temperaturemaintaining the temperature below 25° C. under an atmosphere of argon
2. customThe solution was evaporated
3. customtemperature of 30° C
4. additionThe residual oil was poured, in portions, into saturated aqueous sodium carbonate solution (770 ml)
5. temperaturewhile maintaining the temperature below 30° C
6. extractionThe aqueous mixture was extracted with dichloromethane (3×575 ml)
7. dry with materialdried (Na2SO4)
8. customevaporated