反应详情

The compound (1.00 g, 2.67 mmol) obtained in Step 6 was dissolved in a mixture of acetonitrile (30 ml) and water (10 ml), to which was added CAN (ceric ammonium nitrate) (2.34 g, 4.27 mmol) and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was poured into water and was extracted with ether. After the extract was washed with water and dried, the solvent was distilled off. The residue was purified by a silica gel column chromatography (5% methanol-methylene chloride) and then was crystallized in ethanol/hexane to yield the title compound (662 mg, 1.92 mmol, yield 72%).

1. extractionwas extracted with ether
2. washAfter the extract was washed with water
3. customdried
4. distillationthe solvent was distilled off
5. customThe residue was purified by a silica gel column chromatography (5% methanol-methylene chloride)
6. customwas crystallized in ethanol/hexane