反应详情

The compound (72.7 mg) obtained in Example 43-1 was dissolved in methanol (3.5 ml) and then added with 1-methyl-2-imidazole carboxaldehyde (28.6 mg) and sodium cyanoborohydride (22.8 mg). The reaction solution was adjusted to pH 5 with the addition of acetic acid, followed by stirring at room temperature for 14 hours. The reaction solution was added with a 1 mol/l sodium hydroxide aqueous solution and then extracted with chloroform. Then, the organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. After the solvent had been distilled off, the residue obtained was purified through silica gel column chromatography (chloroform/ethyl acetate) and treated with hydrochloric acid, thereby obtaining hydrochloride (71.3 mg) of the subject compound as a yellow solid.

1. extractionextracted with chloroform
2. washThen, the organic layer was washed with saturated saline solution
3. dry with materialdried with anhydrous sodium sulfate
4. distillationAfter the solvent had been distilled off
5. customthe residue obtained
6. customwas purified through silica gel column chromatography (chloroform/ethyl acetate)
7. additiontreated with hydrochloric acid