反应详情

温度

50 °C

KOtBu (28 mg, 250 μmol) was added at ambient temperature to a solution of 2,5-dichloro-N-{2-[2-(2,5-difluoro-phenyl)-ethoxy]-1-imino-ethyl}-nicotinamide (97 mg, 250 μmol) in DMSO (1 ml). The solution was stirred for 1 h at 50° C., cooled to ambient temperature, KOtBu (28 mg, 250 μmol) was added and the reaction solution was stirred at 50° C. for 14 h. The mixture was poured onto isopropyl acetate/ice water 1/1. The layers were separated and the aqueous layer was extracted two times with isopropyl acetate. The combined extracts were washed three times with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to leave a yellow solid which was recrystallized from dichloromethane/heptane to give 6-chloro-2-[2-(2,5-difluoro-phenyl)-ethoxymethyl]-3H-pyrido[2,3-d]pyrimidin-4-one (8 mg, 23 mmol; 9%) as yellow crystals. MS: m/e=352.3 [M+H+].

1. temperaturecooled to ambient temperature
2. stirringthe reaction solution was stirred at 50° C. for 14 h
3. customThe layers were separated
4. extractionthe aqueous layer was extracted two times with isopropyl acetate
5. washThe combined extracts were washed three times with brine
6. dry with materialdried over sodium sulfate
7. customThe solvent was removed under reduced pressure
8. customto leave a yellow solid which
9. customwas recrystallized from dichloromethane/heptane