反应详情

温度

60 °C

To a mixture of 4-((R)-2-hydroxy-propylamino)-2-methylsulfanyl-pyrimidine-5-carbaldehyde (17.7 g, 78 mmol) and (2,4-difluorophenoxy)acetic acid methyl ester (31.6 g, 156 mmol) in anhydrous dimethyl formamide (300 mL) was added potassium carbonate (30 g, 218 mmol). The reaction mixture was heated to 60° C. and after 18 hours, reaction mixture was cooled and DMF was distilled off. Residue suspended in water (300 mL) and extracted with dichloromethane, washed with brine and dried over magnesium sulfate. Filtered and concentrated under vacuum to give 29.5 g crude material which was chromatographed on silica gel column eluding with 1% methanol in dichloromethane to give 17.5 g 6-(2,4-difluorophenoxy)-8-((R)-2-hydroxypropyl)-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one (mass spec M+1=274).

1. customreaction mixture
2. temperaturewas cooled
3. distillationDMF was distilled off
4. extractionextracted with dichloromethane
5. washwashed with brine
6. dry with materialdried over magnesium sulfate
7. filtrationFiltered
8. concentrationconcentrated under vacuum
9. customto give 29.5 g crude material which
10. customwas chromatographed on silica gel column eluding with 1% methanol in dichloromethane