反应详情

A mixture of 2.5g 4-chloromethyl-1-(3,4-dimethoxybenzyl-6,7-dimethoxyisoquinoline 2-oxide, 35 ml dimethylformamide, 1.8 triethylamine and 1.29 g 1-(2-methoxyphenyl)piperazine was stirred and heated under nitrogen at 50° for 7 hours. After evaporation of the solvent, the residue was partitioned between methylene chloride and water. The methylene chloride solution was washed with water and dried. After removal of the solvent in vacuo, the residue (3.5 g) was crystallized from methylene chloride/ethyl acetate to yield 3.05 g of yellow, hygroscopic crystals of 1-(3,4)-dimethoxybenzyl)-6,7-dimethoxy-4-{]4'-(2-methoxyphenyl)-1'-piperazinyl]methyl} isoquinoline 2-oxide, mp 128°-129° (dec.).

1. temperatureheated under nitrogen at 50° for 7 hours
2. customAfter evaporation of the solvent
3. customthe residue was partitioned between methylene chloride and water
4. washThe methylene chloride solution was washed with water
5. customdried
6. customAfter removal of the solvent in vacuo
7. customthe residue (3.5 g) was crystallized from methylene chloride/ethyl acetate