反应详情

温度

120 °C

A pressure vessel was charged with 8-iodo-3-(3-(methylsulfonyl)propyl)-quinazoline-2,4(1H,3H)-dione (1.09 g, 2.67 mmol), DIEA (1.858 mL, 10.68 mmol) and phosphorus oxychloride (1.222 mL, 13.35 mmol). The tube was sealed and heated in an oil bath at 120° C. for 3 h, then cooled to RT. The solvent was removed in vacuo and the residue was poured into ice/water (50 mL) and 1 M NaOH was added until pH 10. The suspension was filtered and the solid was dried to give the crude product. MS (ESI, pos. ion) m/z: 426.8 (M+1).

1. customThe tube was sealed
2. temperaturecooled to RT
3. customThe solvent was removed in vacuo
4. additionthe residue was poured into ice/water (50 mL) and 1 M NaOH
5. additionwas added until pH 10
6. filtrationThe suspension was filtered
7. customthe solid was dried