反应详情

4-Chloro-6-iodo-3-methanesulfonyl-2-methyl-quinoline (compound of example D.2) (300 mg, 0.786 mmol), (R)-(+)-3-hydroxypiperidine (119 mg, 0.865 mmol) and N,N-diisopropyl ethyl amine (0.148 mL, 0.865 mmol) were heated in dry N,N-dimethylformamide (3 mL) for 0.5 h at 100° C. N,N-Dimethylformamide was evaporated at 40° C./0.1 mbar, the residue was extracted with dichloromethane and 10% Na2CO3, and then purified by chromatography on silica gel in dichloromethane/methanol 20:1. One obtained a yellow oil which was triturated with ethyl acetate and the resulting white crystals were filtered off. One obtained 209 mg (60%) of white crystals. MS: m/z=447 (M+H).

1. customN,N-Dimethylformamide was evaporated at 40° C./0.1 mbar
2. extractionthe residue was extracted with dichloromethane and 10% Na2CO3
3. custompurified by chromatography on silica gel in dichloromethane/methanol 20:1
4. customOne obtained a yellow oil which
5. customwas triturated with ethyl acetate
6. filtrationthe resulting white crystals were filtered off