反应详情

Diethyl phosphorocyanidate (1.2 ml) is added dropwise to a mixture of 7,8-dimethoxy-1,2-dihydro-4-naphthoic acid (0.5 g), 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (0.87 g), triethylamine (0.86 g) and N,N-dimethylformamide (20 ml) with stirring. After stirring for one hour at room temperature, water (100 ml) is added to the reaction mixture and the mixture is extracted with ethyl acetate (100 ml). The organic layer is washed with water, dried and concentrated under reduced pressure. The resulting oily substance is purified by silica gel column chromatography (hexane: acetone=1:1). The product thus obtained is dissolved in ethyl ether and the solution is treated with 5N ethanolic hydrogen chloride (2 ml) to give 1-(7,8-dimethoxy-1,2-dihydro-4-naphthoyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (0.75 g) as colorless powder.

1. stirringAfter stirring for one hour at room temperature
2. extractionthe mixture is extracted with ethyl acetate (100 ml)
3. washThe organic layer is washed with water
4. customdried
5. concentrationconcentrated under reduced pressure
6. customThe resulting oily substance is purified by silica gel column chromatography (hexane: acetone=1:1)
7. customThe product thus obtained