反应详情

Compound 9a, 3.9 g, obtained in Example 1 was heated to reflux for an hour in a solvent mixture of 200 ml of methanol, 50 ml of water and 10 ml of 10 N sodium hydroxide aqueous solution. The solvent was distilled off under reduced pressure and 4 N hydrochloric acid aqueous solution was added to the residue to adjust pH to 7. After concentrating under reduced pressure, the residue was subjected to high porous polymer (HP-10; manufactured by Mitsubishi Chemical Industry Co., Ltd.) column chromatography (eluting solvent; methanol) to give 2.5 g of the crude product. The crude product was recrystallized from water to give 2.0 g of the desired product.

1. temperaturewas heated
2. distillationThe solvent was distilled off under reduced pressure and 4 N hydrochloric acid aqueous solution
3. additionwas added to the residue
4. concentrationAfter concentrating under reduced pressure
5. washthe residue was subjected to high porous polymer (HP-10; manufactured by Mitsubishi Chemical Industry Co., Ltd.) column chromatography (eluting solvent; methanol)
6. customto give 2.5 g of the crude product
7. customThe crude product was recrystallized from water