反应详情

A solution of compound 11 (2.08 g, 4.89 mmol) in acetic acid (15 mL) was refluxed for 4.5 h. The reaction mixture was cooled to rt and concentrated on a rotary evaporator. The residue was dissolved in ethyl acetate and washed with saturated NaHCO3 (2×) and water (1×). The organic layer was dried (MgSO4) and concentrated on a rotary evaporator. The residue was recrystallized from hexane/ethyl acetate to give compound 12 as a tan solid (1.8 g, 90%). ESI-MS m/e 408.3 (M+1).

1. concentrationconcentrated on a rotary evaporator
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with saturated NaHCO3 (2×) and water (1×)
4. dry with materialThe organic layer was dried (MgSO4)
5. concentrationconcentrated on a rotary evaporator
6. customThe residue was recrystallized from hexane/ethyl acetate