反应详情

The compound (413 mg) obtained in Example 2-2 and N-benzyloxycarbonyl-1,4-diaminobutane (247 mg) were dissolved in anhydrous DMF (8.0 ml) and added with WSCI hydrochloride (234 mg) and HOBt (165 mg), followed by stirring at room temperature for 14 hours. After completion of the reaction, the solvent was distilled off. The residue was dissolved in chloroform, washed with 1 mol/l hydrochloric acid, a 1 mol/l sodium hydroxide aqueous solution, and saturated saline solution, and dried with anhydrous magnesium sulfate, followed by distilling the solvent off. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol/water) and treated with hydrochloric acid, thereby obtaining hydrochloride (23.0 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 dissolved in chloroform
4. washwashed with 1 mol/l hydrochloric acid
5. dry with materiala 1 mol/l sodium hydroxide aqueous solution, and saturated saline solution, and dried with anhydrous magnesium sulfate
6. distillationby distilling the solvent off
7. customSubsequently, the residue was purified through silica gel column chromatography (chloroform/methanol/water)
8. additiontreated with hydrochloric acid