反应详情

A solution of 4-acetylphenyl isocyanate (1.61 g; 10 mmole) in methylene chloride (100 ml) was added to a solution of 1-(3-aminopropyl)-4-(4-chlorobenzyl)piperazine trihydrochloride (3.77 g; 10 mmole), methylene chloride (50 ml) and triethylamine (4.3 ml; 31 mmole). The resulting mixture was refluxed 3 hours, washed with aqueous sodium bicarbonate, dried (sodium sulfate), and the product precipitated with ethereal hydrochloric acid. Recrystallization from ethanol provided the title compound (4.13 g; 82% yield) as a white powder, m.p. >197° C. (slow dec.).

1. temperatureThe resulting mixture was refluxed 3 hours
2. washwashed with aqueous sodium bicarbonate
3. dry with materialdried (sodium sulfate)
4. customthe product precipitated with ethereal hydrochloric acid
5. customRecrystallization from ethanol