反应详情

29 ml (46.5 mmol) of a 15% strength butyllithium solution in n-hexane were slowly added dropwise to a stirred solution of 9.26 g (46.5 mmol) of N,N-bis(trimethylsilyl)-2-propynylamine from stage C1 in 50 ml of tetrahydrofuran at -40° C. under argon. The mixture was then warmed to room temperature and again cooled to -40° C., and a solution of 14.25 g (46.5 mmol) of 3-methyl-1-(5-oxohexyl)-7-propylxanthine in 40 ml of tetrahydrofuran was slowly added. After removal of the cooling bath, the mixture was stirred at room temperature for 6 hours. The reaction mixture was then added to saturated ammonium chloride solution at 0° C., the aqueous phase was extracted with ether, the organic phase was dried over sodium sulfate, the desiccant was filtered off, and the solvent was removed under reduced pressure. The crude product was subjected to flash chromatography first with the mobile phase mixture dichloromethane/methanol/saturated ammonia solution=19/1.5/2.5 and then with 9/1/2.5. Yield: 9.79 g (58% of theory); yellowish oil

1. temperatureagain cooled to -40° C.
2. customAfter removal of the cooling bath
3. additionThe reaction mixture was then added to saturated ammonium chloride solution at 0° C.
4. extractionthe aqueous phase was extracted with ether
5. dry with materialthe organic phase was dried over sodium sulfate
6. filtrationthe desiccant was filtered off
7. customthe solvent was removed under reduced pressure