反应详情

The compound (190 mg) obtained in Example 2-2 was dissolved in DMF (3.0 ml) and added with DCC (189 mg), HOBt (124 mg), and the compound (96.9 mg) obtained in Example 22-3, 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, followed by separating the solution into layers by the addition of 1 mol/l hydrochloric acid. The aqueous layer was made basic with a 1 mol/l sodium hydroxide aqueous solution. Then, the solution was subjected to extraction with chloroform. The extract was washed with saturated saline solution and the organic layer was then dried with anhydrous sodium sulfate. The solvent was distilled off. Subsequently, the residue was treated with hydrochloric acid and then purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining hydrochloride (84.8 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. customby separating the solution into layers
5. additionby the addition of 1 mol/l hydrochloric acid
6. extractionThen, the solution was subjected to extraction with chloroform
7. washThe extract was washed with saturated saline solution
8. dry with materialthe organic layer was then dried with anhydrous sodium sulfate
9. distillationThe solvent was distilled off
10. additionSubsequently, the residue was treated with hydrochloric acid
11. custompurified through silica gel column chromatography (chloroform/methanol/water)