反应详情

The compound obtained in Example 11-5 (30.6 mg) was dissolved in methanol (0.7 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.7 ml) was added. The mixture was stirred for 3 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with an aqueous solution of hydrochloric acid, concentrated and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (22.7 mg) as a white solid.

1. customAfter the reaction
2. customthe solvent was removed by distillation
3. customThe residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
4. additionThe obtained product was added with an aqueous solution of hydrochloric acid
5. concentrationconcentrated
6. distillationazeotropically distilled with water
7. washThe resulting solid was washed with ether