反应详情

A solution of 2,3-dimethoxy-6,7-dihydro-5H-benzocycloheptene-8-carbonyl chloride (0.36 g) in dichloromethane (6 ml) is added dropwise, at 0° C. while stirring, to a mixture of 3-methoxymethyl-1-(3,4,5trimethoxybenzyl)piperazine (0.4 g) obtained in Reference Example 14, triethylamine (0.3 g) and dichloromethane (6 ml). After stirring at room temperature for one hour, the reaction mixture is added to water, followed by extraction with dichloromethane. The organic layer is washed with water and dried, then the solvent is distilled off under reduced pressure. The residue is purified by means of a silica gel column chromatography (hexane:ethyl acetate:acetone=2:2:1) to afford 1-(2,3-dimethoxy-6,7-dihydro-5H-benzo-cyclohepten-8-ylcarbonyl) -2-methoxymethyl-4-(3,4,5-tri-methoxybenzyl)piperazine (0.6 g) as a colorless oily product. This product is converted to the hydrochloride, and treated with ethyl ether to give pale yellow powder.

1. extractionfollowed by extraction with dichloromethane
2. washThe organic layer is washed with water
3. customdried
4. distillationthe solvent is distilled off under reduced pressure
5. customThe residue is purified by means of a silica gel column chromatography (hexane:ethyl acetate:acetone=2:2:1)