反应详情

The compound (100 mg) obtained in Example 2-2 was dissolved in DMF (2.0 ml) and then added with DCC (55.4 mg), HOBt (36.3 mg), and the compound (50.0 mg) obtained in Example 23-3, followed by stirring overnight at room temperature. After completion of the reaction, the solvent was distilled off and the residue was then dissolved in chloroform. Then, the solution was added with 1 mol/l hydrochloric acid to separate the solution into layers. After the aqueous layer was added with a 1 mol/l sodium hydroxide aqueous solution to make the solution basic, the solution was subjected to extraction with chloroform and the extract was then washed with saturated saline solution. Subsequently, the organic layer was dried with anhydrous sodium sulfate. The solvent was distilled off and the residue was then treated with hydrochloric acid. After that, the residue was subjected to purification through silica gel column chromatography (chloroform/methanol/water), thereby obtaining hydrochloride (17.5 mg) of the subject compound as a white solid.

1. customAfter completion of the reaction
2. distillationthe solvent was distilled off
3. dissolutionthe residue was then dissolved in chloroform
4. additionThen, the solution was added with 1 mol/l hydrochloric acid
5. customto separate the solution into layers
6. additionAfter the aqueous layer was added with a 1 mol/l sodium hydroxide aqueous solution
7. extractionthe solution was subjected to extraction with chloroform
8. washthe extract was then washed with saturated saline solution
9. dry with materialSubsequently, the organic layer was dried with anhydrous sodium sulfate
10. distillationThe solvent was distilled off
11. additionthe residue was then treated with hydrochloric acid
12. customAfter that, the residue was subjected to purification through silica gel column chromatography (chloroform/methanol/water)