反应详情

4-geranyloxybenzoic acid(1.92 g) was dissolved in chloroform(50 ml) and triethylamine(1.95 ml), and then diphenylphosphinic chloride(1.34 ml) was added thereto while being cooled with ice. After being stirred for 1 hour, the mixture, with 2-(2-aminoethylamino)-5-methoxypyridine(1.17 g) added thereto, was stirred for 8 hours at room temperature. The reaction mixture was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively, dried over sodium sulfate anhydride, and then concentrated under a vacuum. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1). The resulting solid was recrystallized from n-hexane/ethyl acetate, thereby yielding 2.22 g of the aimed compound.

1. temperaturewhile being cooled with ice
2. stirringwas stirred for 8 hours at room temperature
3. washThe reaction mixture was washed with saturated sodium hydrogencarbonate aqueous solution and saturated brine successively
4. dry with materialdried over sodium sulfate anhydride
5. concentrationconcentrated under a vacuum
6. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
7. customThe resulting solid was recrystallized from n-hexane/ethyl acetate