反应详情

A solution of N-[(4aR,7aS)-7a-phenyl-4a,5,6,7-tetrahydro-4H-pyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide (250 mg, 0.629 mmol), 5-fluoro-2-chloropyrimidine (167 mg, 1.26 mmol), 1,4-dioxane (10 mL), and triethylamine (318 mg, 3.14 mmol) is stirred at 110° C. for 4 hours. The reaction is cooled, diluted with water and extracted with dichloromethane. The organic layers are combined, dried, filtered, and concentrated under reduced pressure to give a residue. The residue is purified by silica gel flash chromatography, eluting with hexane/ethyl acetate (1:0) to hexane/ethyl acetate (0:1) to give the title compound (0.217 g, 80%). ES/MS (m/e): 434(M+H).

1. temperatureThe reaction is cooled
2. extractionextracted with dichloromethane
3. customdried
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customto give a residue
7. customThe residue is purified by silica gel flash chromatography
8. washeluting with hexane/ethyl acetate (1:0) to hexane/ethyl acetate (0:1)