反应详情

The compound (28.8 mg) obtained in Example 3-2 was dissolved in methanol (0.5 ml). The solution was added with cyclohexanone (8.80 μl) and sodium cyanoborohydride (4.40 mg) and then adjusted to approximately pH 5 with acetic acid, followed by stirring at room temperature for 16 hours. After completion of the reaction, the solvent was distilled off. Then, the residue was dissolved in chloroform and washed with a 1 mol/l sodium hydroxide aqueous solution and saturated saline solution, followed by the addition of 1 mol/l hydrochloric acid to extract the objective substance. Subsequently, the aqueous layer was concentrated under reduced pressure and then the residue was purified through a solid-phase extraction column (Bond Elut® C18 (manufactured by Varian Inc.), 200 mg), thereby obtaining hydrochloride (17.6 mg) of the subject compound as a white solid.

1. customAfter completion of the reaction
2. distillationthe solvent was distilled off
3. dissolutionThen, the residue was dissolved in chloroform
4. washwashed with a 1 mol/l sodium hydroxide aqueous solution and saturated saline solution
5. additionfollowed by the addition of 1 mol/l hydrochloric acid
6. extractionto extract the objective substance
7. concentrationSubsequently, the aqueous layer was concentrated under reduced pressure
8. customthe residue was purified through a solid-phase extraction column (Bond Elut® C18 (manufactured by Varian Inc.), 200 mg)