反应详情

温度

135 °C

1-(4-Bromophenyl)-2-mercapto-9-methyl-1,9-dihydro-6H-purin-6-one hydrochloride (2.05 g, 5.49 mmol) is added to POCl3 (87 mL) and the resulting solution is refluxed at 135° C. for 38 h. Most volatiles are removed under vacuum and the residual solvents are co-evaporated with toluene (50 mL×3). The resulting dark solid is dissolved in CH2Cl2 (300 mL), washed with saturated NaHCO3 solution (100 mL×5), brine (50 mL×2), and dried over MgSO4. After removing solvent in vacuo, silica gel column chromatography (EtOAc:hexanes=50:50) gives the title compound as a yellow solid. 1H NMR (400 MHz, CDCl3) 7.51 (1H, s), 7.67 (2H, d), 7; 14 (2H, d), 3.83 (3H, s); m/z (ES+) 340.90 (M+).

1. customMost volatiles are removed under vacuum
2. dissolutionThe resulting dark solid is dissolved in CH2Cl2 (300 mL)
3. washwashed with saturated NaHCO3 solution (100 mL×5), brine (50 mL×2)
4. dry with materialdried over MgSO4
5. customAfter removing solvent in vacuo, silica gel column chromatography (EtOAc:hexanes=50:50)