反应详情

The product from Step 1 (0.762 g, 1.76 mmol, 1.00 equiv) was dissolved in MeOH (20 mL) and NaOH (2.0 M, 3.5 mL) and the mixture was heated to reflux for 1.5 hours. The reaction was cooled to room temperature and concentrated en vacuo. The residue was dissolved in H2O and 6N HCl was added to acidify the solution to pH 1. The crystalline precipitate was isolated by filtration, washed with H2O and air dried. The residue was further dried en vacuo to provide 0.586 g (80%) of the product as an amorphous solid. MS (ES+) m/e 420 [M+H]+

1. temperatureto reflux for 1.5 hours
2. concentrationconcentrated en vacuo
3. dissolutionThe residue was dissolved in H2O
4. addition6N HCl was added
5. customThe crystalline precipitate was isolated by filtration
6. washwashed with H2O and air
7. customdried
8. customThe residue was further dried en vacuo