反应详情

Combine 1-benzyl-4-(4-fluoro-phenylamino)-piperidine-4-carbonitrile (32 mmol) and dichloromethane (100 mL). Add chlorosulfonyl isocyanate (20 mmol) in dropwise fashion with water bath cooling so as to maintain the temperature of the reaction mixture between 20° and 30° C. After 30 minutes, concentrate the reaction mixture in vacuo to obtain a residue. Add 1N HCl (100 mL) and heat at reflux for 1 h. Cool in an ice bath and adjust the pH to 5.5 using 5N NaOH. Filter to obtain a residue. Wash with diethyl ether and dry in vacuo. Purify to obtain the title compound.

1. temperatureto maintain the temperature of the reaction mixture between 20° and 30° C
2. concentrationconcentrate the reaction mixture in vacuo
3. customto obtain a residue
4. temperatureheat
5. temperatureat reflux for 1 h
6. temperatureCool in an ice bath
7. filtrationFilter
8. customto obtain a residue
9. washWash with diethyl ether
10. customdry in vacuo
11. customPurify