反应详情

Combine 8-benzyl-1-(4-fluoro-phenyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione (10 mmol) and 1,2-dichloroethane (70 mL). Cool using an ice bath. Add in dropwise fashion, 1-chloroethyl chloroformate (48.6 mmol). Warm to ambient temperature and maintain for 1 h. Extract using saturated NaHCO3 (120 mL). Extract the aqueous phase using dichloromethane (120 mL). Combine the organic layers, extract with saturated NaCl, dry over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Add anhydrous methanol (70 mL) and heat at reflux for 1 h. Concentrate in vacuo to obtain a residue and purify to obtain the title compound.

1. temperatureCool
2. temperaturemaintain for 1 h
3. extractionExtract
4. extractionExtract the aqueous phase
5. extractionCombine the organic layers, extract with saturated NaCl
6. dry with materialdry over Na2SO4
7. filtrationfilter
8. concentrationconcentrate in vacuo
9. customto obtain a residue
10. temperatureat reflux for 1 h
11. concentrationConcentrate in vacuo
12. customto obtain a residue
13. custompurify