反应详情

A mixture of 6-bromo-7-(1-bromoethyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one (11.1 g, 31.5 mmol) and sodium azide (6.15 g, 94.6 mmol) in dimethyl formamide (DMF) (100 mL) was stirred at room temperature for 2 h. After diluting with EtOAc, the mixture was washed with water, brine, dried over sodium sulfate, and evaporated under reduced pressure. The crude residue was purified on silica gel, eluting with 0 to 80% EtOAc in hexane, to provide the product (8.68 g, 87.6%). LCMS calculated for C9H9BrN5OS (M+H)+: m/z=314.0. Found: 313.9. 1H NMR (DMSO-d6, 300 MHz) δ 7.15 (1H, s), 4.83 (1H, q, J=6.6 Hz), 2.69 (3H, s), 1.48 (3H, d, J=6.6 Hz) ppm.

1. washthe mixture was washed with water, brine
2. dry with materialdried over sodium sulfate
3. customevaporated under reduced pressure
4. customThe crude residue was purified on silica gel
5. washeluting with 0 to 80% EtOAc in hexane