反应详情

The compound obtained in Example 87-2 (1 g) was dissolved in methanol (25 ml). The solution was stirred for 15 hours while blowing hydrochloric acid gas, and the solvent was removed by distillation. The obtained residue was dissolved in water and 1 mol/l sodium hydroxide aqueous solution was added to cause a solid substance to precipitate. The solid was collected by filtration and the filtrate was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was removed by distillation to obtain a solid. The solid was combined with the previously collected solid and purified by silica gel column chromatography (20 g, chloroform) to obtain the title compound (0.7337 g) as a white solid.

1. customthe solvent was removed by distillation
2. dissolutionThe obtained residue was dissolved in water
3. addition1 mol/l sodium hydroxide aqueous solution was added
4. customto precipitate
5. filtrationThe solid was collected by filtration
6. extractionthe filtrate was extracted with chloroform
7. dry with materialThe extract was dried over anhydrous sodium sulfate
8. customthe solvent was removed by distillation
9. customto obtain a solid
10. custompurified by silica gel column chromatography (20 g, chloroform)