Sodium hydride → HCID 24887948, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 0.226 g (0.88 mmol) of 8,8-dimethyl-2-(pyridin-4-yl)-6,7,8,9-tetrahydro-pyrimido[1,2-a]pyrimidin-4-one in 5 ml of anhydrous dimethylformamide was added 0.040 g (0.97 mmol) of sodium hydride (60% suspension in mineral oil) and the mixture was allowed to stir at 45° C. for 3 hours. 0.20 g (0.88 mmol) of methanesulfonic acid 6,7-dihydro-5H-[1]pyrindin-6-(R)-ylmethyl ester was added and the stirring continued at 80° C. for 18 h. The mixture was cooled and a solution of saturated ammonium chloride was added. The mixture was extracted with trichloromethane/methanol 90/10. The extracts were washed with a saturated aqueous solution of sodium chloride, dried and evaporated to give crude product. Purification by chromatography on silica gel eluting with a mixture of ethyl acetate/ethanol in the proportions 100/0 to 70/20, gives 0.197 g (58%) of the compound in the form of free base. Mp.: 202-204° C.

Provenance & Evidence