反应详情

A suspension of 5-(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (130 mg, 0.55 mmol, 1 eq) and KOH, 85% (1.2 eq, 44 mg) in 5 ml of absolute ethanol was stirred with ultrasound bath at room temperature for 1 hour. In the suspension was then added MeI (1.2 eq, 42 μl) dropwise and the mixture was stirred in a sealed vial at 70° C. (temperature on display of heating device) for 20 hours (overnight). The solvent was then evaporated. In the crude was added 10 ml of water and pH of the solution was adjusted to 7-7.5. The resulting suspension was filtered over filter paper. The filtrate was washed with chloroform (3 times, 30 ml was used in total). pH of the water layer was adjusted to 5-5.5 and using ultrasound bath precipitate was formed. The precipitate was collected, it was dried and obtained was 2-methylsulfanyl-5-(6-oxo-1,6-dihydro-pyridin-3-ylmethyl)-1H-pyrimidin-4-one (22 mg, yield=15.9%, purity=95%) in form of white powder. MS: [M+H]+=250.18 1H NMR (300 MHz; DMSO-d6) δ/ppm 2.46 (s, 3H), 3.31 (s, 2H), 6.25 (d, J=9.37 Hz, 1H), 7.19 (d, J=2.06 Hz, 1H), 7.35 (dd, J=9.37 Hz, J=2.45 Hz, 1H), 7.77 (s, 1H)

1. temperaturesealed vial at 70° C. (temperature on display of heating device) for 20 hours (overnight)
2. customThe solvent was then evaporated
3. additionIn the crude was added 10 ml of water and pH of the solution
4. filtrationThe resulting suspension was filtered
5. filtrationover filter paper
6. washThe filtrate was washed with chloroform (3 times, 30 ml was used in total)
7. customwas formed
8. customThe precipitate was collected
9. customit was dried
10. customobtained