反应详情

温度

85 °C

Combine the 2-[3-(3,4-dichloro-phenyl)-1-(3,4,5-trimethoxy-benzoyl)-pyrrolidin-3-yl]-ethyl-methanesulfonate (5.0 mmol), 1-(4-fluoro-phenyl)-1,3,8-triaza-spiro[4.5]decane-2,4-dione hydrochloride (7.5 mmol, 1.5 eq.), N,N-diisopropylethylamine (15 mmol), and DMF (8 mL). Heat the mixture at 85° C. for 48 h. Cool to ambient temperature and add ethyl acetate (100 mL). Extract with water (25 mL), 1N HCl (2×25 mL), saturated NaHCO3 (25 mL), and saturated NaCl (25 mL). Dry over MgSO4, filter, and concentrate in vacuo to obtain a residue. Purify to obtain the title compound.

1. temperatureCool to ambient temperature
2. extractionExtract with water (25 mL), 1N HCl (2×25 mL), saturated NaHCO3 (25 mL), and saturated NaCl (25 mL)
3. dry with materialDry over MgSO4
4. filtrationfilter
5. concentrationconcentrate in vacuo
6. customto obtain a residue
7. customPurify