反应详情

Diethyl phosphorocyanidate (0.9 g) is added dropwise to an ice-cooling mixture consisting of 5,6-dimethoxy-1H-indene-2-carboxylic acid (0.8 g), 1-(3,4,5-trimethyoxybenzyl)piperazine dihydrochloride (1.3 g), triethylamine (2 ml) and N,N-dimethylformamide (12 ml) with stirring. The whole mixture is stirred at room temperature for two hours and water is added. The mixture is extracted with ethyl acetate. The extract solution is washed with water, dried and then concentrated under reduced pressure. The residue is purified by silica gel column chromatography (ethyl acetate:hexane:acetone=12:8:5) to give an oily product. This product is converted to the hydrochloride in ethanol to afford 1-(5,6-dimethoxy-1H-inden-2-ylcarbonyl)-4-(3,4,5-trimethoxybenzyl)piperazine hydrochloride (1.45 g) as colorless scales, m.p. 245°-250° C. (decomp.).

1. temperaturecooling mixture
2. stirringThe whole mixture is stirred at room temperature for two hours
3. extractionThe mixture is extracted with ethyl acetate
4. washThe extract solution is washed with water
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe residue is purified by silica gel column chromatography (ethyl acetate:hexane:acetone=12:8:5)
8. customto give an oily product