反应详情

A solution of 4-methoxy cinnamoyl chloride (0.3 g) in dichloromethane (4 ml) is added dropwise, taking 3 minutes at 0 ° C while stirring, to a mixture of methyl 1-(3,4,5-trimethoxybenzoyl)piperazine-2-carboxylate (0.57 g), triethylamine (0.4 g) and dichloromethane (12 ml). The reaction mixture is stirred for 30 minutes at room temperature, and then poured into water, followed by extraction with dichloromethane. The organic layer is washed with dilute hydrochloric acid, an aqueous solution of sodium hydrogencarbonate and water, successively, then the solvent is distilled off. The residue is purified by means of a silica gel column chromatography to give methyl 4-(4-methoxycinnamoyl)-1(3,4,5-trimethoxybenzoyl)piperazine-2-carboxylate (0.6 g) as a colorless oily product. This product is processed with ethyl ether to give colorless powder

1. extractionfollowed by extraction with dichloromethane
2. washThe organic layer is washed with dilute hydrochloric acid
3. distillationan aqueous solution of sodium hydrogencarbonate and water, successively, then the solvent is distilled off
4. customThe residue is purified by means of a silica gel column chromatography