反应详情

A solution of Intermediate 85f (2.50 g, 7.93 mmol) and lithium hydroxide monohydrate (3.33 g, 79.3 mmol) in MeOH and water (50 mL) was stirred at reflux for 2 h. The cooled solution was acidified with 1M HCl to pH 5. The MeOH was removed in vacuo and the resulting aqueous layer was extracted with EtOAc (3×). The combined organic layers were dried (MgSO4) and concentrated in vacuo to give the title compound as a white foam (2.21 g, 92%). 1H NMR (400 MHz, CDCl3): 1.00-1.21 (21H, m), 1.93-2.04 (2H, m), 2.32-2.42 (1H, m), 2.43-2.56 (1H, m), 2.96-3.09 (4H, m), 3.90-4.00 (1H, m), 4.20 (1H, d, J 10.9), 4.22 (1H, d, J 10.9).

1. temperatureat reflux for 2 h
2. customThe MeOH was removed in vacuo
3. extractionthe resulting aqueous layer was extracted with EtOAc (3×)
4. dry with materialThe combined organic layers were dried (MgSO4)
5. concentrationconcentrated in vacuo