反应详情

To a stirred solution of 7-(1-azidoethyl)-6-(3-fluorophenyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one (0.14 g, 0.42 mmol) (1st peak from chiral separation) in tetrahydrofuran (3 mL) and water (0.5 mL) was added 1.00 M of trimethylphosphine in tetrahydrofuran (0.52 mL, 0.52 mmol), and the mixture was stirred at room temperature for 1 hour. To the mixtures were added ethyl acetate and the mixtures were extracted with aqueous 1 N HCl solution (three times). The combined extracts were neutralized with solid NaHCO3, and extracted with dichloromethane (three times). The combined organic layers were washed with brine, dried over MgSO4, and concentrated to give the crude product (0.125 g) used directly in next step. LCMS calculated for C15H15FN3OS (M+H)+: m/z=304.1. Found: 304.0.

1. extractionthe mixtures were extracted with aqueous 1 N HCl solution (three times)
2. extractionextracted with dichloromethane (three times)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated