Hydrochloric Acid → HCID 19898731, compound

Participants

Reaction Steps

In 50 ml of dioxane, there were heated under reflux 1.78 g of the previously obtained, 3-(3-methyl-4-oxo-4H-1-benzopyran-5-yl)oxypropyl bromide (Compound 2), 1.34 g of 1,3-dimethyl-6-(piperazine-1-yl)-2,4(1H,3H)-pyrimidinedione (Compound 3) and 1.5 ml of triethylamine for 2 hours. After cooling and then filtration, the resultant filtrate was concentrated under reduced pressure, and the resultant residue was then dissolved in chloroform, washed with water, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. The thus obtained residue was purified through a silica gel column chromatograph (chloroform:methanol=100:2 to 100:10 in volume ratio) and then recrystallized from ethanol and ether in order to obtain 2.40 g (yield 91%) of 1,3-dimethyl-6-(4-[3-(3-methyl-4-oxo-4H-1-benzopyran-5-yl)oxypropyl]piperazine-1-yl)-2,4(1H,3H)-pyrimidinedione (the non-hydrochloride of Compound 4).

Provenance & Evidence