反应详情

1.9 g (6.2 mmol) of ethyl N-(3-carboethoxy-6-methyl-4,5,6,7-tetrahydrothieno[2,3-c]pyridin-2-yl)ethanimidate in 30 ml of ethanol were mixed with 1.5 g (6.2 mmol) of 1-(2-aminoethyl)-4-(2-methoxyphenyl)piperazine and refluxed for 7 h. The mixture was then concentrated in a rotary evaporator, and the residue was taken up in 20 ml of ethyl acetate. 2.1 g of crude product crystallized out overnight and were filtered off with suction and purified by column chromatography (silica gel, mobile phase methylene chloride/methanol 92/8). 0.8 g (29%) of product was isolated.

1. temperaturerefluxed for 7 h
2. concentrationThe mixture was then concentrated in a rotary evaporator
3. custom2.1 g of crude product crystallized out overnight
4. filtrationwere filtered off with suction
5. custompurified by column chromatography (silica gel, mobile phase methylene chloride/methanol 92/8)