反应详情

A mixture of compound 9a (8.90 g, 14 mmol) and formic acid (15 mL, 96% in H2O) in EtOH (150 mL) was refluxed for 24 h. After cooling, the solution was concentrated in vacuo. The residue was subjected to a short column using EtOAc in hexane (30% to 70%) to give the crude compound 10a which was triturated with 10% EtOAc in hexane to give compound 10a (4.50 g, 87% yield). 1H NMR (500 MHz, CDCl3) δ 1.17 (s, 9H), 5.09 (s, 2H), 7.20-7.39 (m, 5H), 8.01 (s, 1H), 8.84 (s, 1H).

1. temperaturewas refluxed for 24 h
2. temperatureAfter cooling
3. concentrationthe solution was concentrated in vacuo
4. customto give the crude compound 10a which
5. customwas triturated with 10% EtOAc in hexane