反应详情

温度

80 °C

A mixture of 2-(1-bromopropyl)-6-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.46 g, 12.3 mmol) and N-iodosuccinimide (4.15 g, 18.4 mmol) in acetonitrile (100 mL) was stirred at 80° C., under nitrogen, overnight. After removal of acetonitrile in vacuum, the resulting solid was dissolved in methylene chloride, washed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine; and then the organic layers dried over sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to provide the desired product (4.53 g, 90.4%). LCMS calculated for C12H13BrIN2O (M+H)+: m/z=406.9. Found: 407.1.

1. customAfter removal of acetonitrile in vacuum
2. dissolutionthe resulting solid was dissolved in methylene chloride
3. washwashed with water, saturated Na2S2O3, saturated sodium bicarbonate, and brine
4. dry with materialand then the organic layers dried over sodium sulfate
5. filtrationfiltered
6. concentrationThe filtrate was concentrated under reduced pressure