反应详情

Hydrogen chloride is bubbled into a solution of 81 (110 mg, 0.25 mmol) in EtOAc (10 mL) for 1 min, and the solution is stirred at RT for 6 h. The solvent is removed by rotary evaporation, and the residue triturated with Et2O. The insoluble material is dissolved in dichloromethane and Et2O is added, and the precipitate is filtered to give 43 mg of the product 82. 1H NMR (DMSO-d6) δ 9.28 (s, 2 H), 7.60-7.30 (m, 5 H), 7.25-6.95 (m, 10 H), 5.58 (s, 2 H), 4.78 (s, 2 H), 3.15 (s, 3 H); MS: m/z 342 (M++1).

1. customThe solvent is removed by rotary evaporation
2. customthe residue triturated with Et2O
3. dissolutionThe insoluble material is dissolved in dichloromethane
4. additionEt2O is added
5. filtrationthe precipitate is filtered