反应详情

To 6-Piperidin-1-yl-1H-quinazoline-2,4-dione (522 mg, 2.13 mmol) and triethyl amine hydrochloride (1.2 g, 8.5 mmol) was added POCl3 (20 mL) and the solution was heated to 120 C for 72 h. POCl3 was removed in vacuum and the resulting brown oil was quenched with ice water and treated with saturated NaHCO3, to afford a tan solid. Filtration and drying in vacuum gave title compound 550 mg (91% yield). HPLC tr=8.56 min (100%), FIA m/z 282.1 (M+H), HNMR (500 MHz, dmso): δ 8.05–8.00 (1H, d), 7.85–7.80 (1H, d), 7.20 (1H s), 5.50–4.40 (4H, m), 1.70–1.60 (6H, m).

1. temperaturethe solution was heated to 120 C for 72 h
2. customPOCl3 was removed in vacuum
3. customthe resulting brown oil was quenched with ice water
4. additiontreated with saturated NaHCO3
5. customto afford a tan solid
6. filtrationFiltration
7. customdrying in vacuum