反应详情

Triphenyl phosphine(102 mg) and diethyl azodicarboxylate(68 mg) were added to a tetrahydrofuran (THF) solution(5 ml) of 4-hydroxy-1-methyl-1H-quinolin-2-one(63 mg), and 3-[(2-pyridin-3-ylethyl)pyridin-4-ylmethylamino]propane-1-ol(81.4 mg). The mixture was stirred overnight. After the reaction mixture was condensed under reduced pressure, the residue was purified by silica gel column chromatography (dichloromethane: methanol=20:1→10:1). The purified product was condensed under reduced pressure. A 4N-hydrogen chloride ethyl acetate solution(0.29 ml) was added to an ethyl acetate solution of the residue, which was stirred at room temperature for 30 minutes. The generated insoluble matter was separated by filtration, and dried to give the title compound(126.8 mg) as a white powder.

1. customcondensed under reduced pressure
2. customthe residue was purified by silica gel column chromatography (dichloromethane: methanol=20:1→10:1)
3. customcondensed under reduced pressure
4. stirringwas stirred at room temperature for 30 minutes
5. customThe generated insoluble matter was separated by filtration
6. customdried