反应详情

A solution of PMW04140 (3.37 g, 16.7 mmol) in MeOH (70 mL) containing conc. HCl (15 drops) was heated at reflux overnight. The mixture was allowed to cool and was neutralised with sat aq. NaHCO3. The solvent was removed in vacuo and the residue was dissolved in EtOAc (100 mL) and washed with H2O (100 mL), sat. aq, NaHCO3 (100 mL) and brine (100 mL) then dried (MgSO4) and the solvent was removed in vacuo. The title compound (3.30 g, 92%) was obtained as a pale yellow oil; 1H NMR. (270 MHz, DMSO-d6) 3.61 (2H, s, CH2), 3.69 (3H, s, CH3), 3.76 (3H, s, CH3), 6.40-6.49 (2H, m, ArH); 19F NMR (376.4 MHz, DMSO-d6)-114.4 (d); HRMS (ES+) calcd, for C10H11F2O3 (M++H) 217.0657. found 217.0663; LC/MS (ES+) tr=1.69 min, m/z 216.8 (M+, 100%).

1. temperaturewas heated
2. temperatureat reflux overnight
3. temperatureto cool
4. customThe solvent was removed in vacuo
5. dissolutionthe residue was dissolved in EtOAc (100 mL)
6. washwashed with H2O (100 mL)
7. dry with materialsat. aq, NaHCO3 (100 mL) and brine (100 mL) then dried (MgSO4)
8. customthe solvent was removed in vacuo