反应详情

温度

0 °C

A mixture of 0.084 g (0.28 mmol) of the product (24) from Step 8 and 0.08 mL (0.56 mmol) of triethylamine in 2.5 mL of anhydrous DCM was cooled to 0° C. Then was added dropwise 0.03 mL (0.34 mmol) of methanesulfonyl chloride and the resulting mixture was allowed to warm to ambient temperature under nitrogen. Excess DCM was added and the reaction mixture was washed with water, saturated NaHCO3 and brine. The organic layer was then dried over MgSO4 and the solvent was removed in vacuo yielding 0.106 g (0.28 mmol, 100%) of 1-(3-benzyl-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidin-2-yl)propyl methanesulfonate (25) as a tan oil.

1. temperatureto warm to ambient temperature under nitrogen
2. washthe reaction mixture was washed with water, saturated NaHCO3 and brine
3. dry with materialThe organic layer was then dried over MgSO4
4. customthe solvent was removed in vacuo