反应详情

To a THF (3.8 mL) solution of the compound (3.832 g) obtained in Example 9-(2), H3PO4 (6.1 mL, 85% aqueous solution) was added and the mixture was stirred at room temperature for an hour. To the reaction mixture, THF (50 mL) was added and the resulting mixture was added to NaOH (150 mL, 1.0 N aqueous solution) and ice (50 g), followed by extraction with CHCl3 (300 mL). The organic layer was dried (Na2SO4), filtered and concentrated to give a crude product, which was further purified by NH-form silica gel chromatography (MeOH/CHCl3) to give the titled compound (1.261 g, colorless oil.)

1. extractionfollowed by extraction with CHCl3 (300 mL)
2. dry with materialThe organic layer was dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a crude product, which
6. customwas further purified by NH-form silica gel chromatography (MeOH/CHCl3)