反应详情

To a solution of 4- geranyloxybenzoic acid (1.10 g) in chloroform (20 ml), triethylamine (1.11 ml) and a solution of diphenylphosphinic chloride (0.95 g) in chloroform (5 ml) were successively added. After the reaction solution was stirred for 30 minutes, 4-amino-1,2-diethylpyrazolidine (0.57 g) was added and then the mixture was stirred at room temperature for one night. The reaction solution was washed with aqueous solution of sodium hydrogencarbonate, dried over sodium sulfate anhydride, and then concentrated under a vacuum. The residue was purified by silica gel column chromatography (chloroform:methanol=20:1) and then recrystallized from n-hexane, thereby yielding 1.39 g (87%) of the aimed compound.

1. stirringthe mixture was stirred at room temperature for one night
2. washThe reaction solution was washed with aqueous solution of sodium hydrogencarbonate
3. dry with materialdried over sodium sulfate anhydride
4. concentrationconcentrated under a vacuum
5. customThe residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
6. customrecrystallized from n-hexane