反应详情

A mixture of 9-oxo-2-fluorene carboxylic acid (1 g), toluene (10 ml), and thionyl chloride (3 ml) is heated for one hour under reflux. The mixture is evaporated to dryness. To the residue is added toluene (10 ml), and the mixture is again evaporated to dryness. Thus-obtained yellow powder is mixed with toluene (50 ml), and the mixture is added to a mixture of 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (1.8 g), triethylamine (4.3 g) and N,N-dimethylformamide (20 ml). The resulting mixture is left standing at room temperature for 30 minutes and treated with water (300 ml). The whole mixture is extracted with ethyl acetate (500 ml). The organic layer is washed with water, dried and concentrated to afford 1-(9-oxo-2-fluorenylcarbonyl)-4-(3,4,5-trimethoxybenzyl)piperazine (1.1 g) as pale yellow crystals, m.p. 166°-168° C.

1. temperatureis heated for one hour
2. temperatureunder reflux
3. customThe mixture is evaporated to dryness
4. additionTo the residue is added toluene (10 ml)
5. customthe mixture is again evaporated to dryness
6. customThus-obtained yellow powder
7. waitThe resulting mixture is left
8. extractionThe whole mixture is extracted with ethyl acetate (500 ml)
9. washThe organic layer is washed with water
10. customdried
11. concentrationconcentrated