反应详情

A mixture of 1-(3-chloropropyl)-3-(4-cyanophenyl)urea (3.57 g; 15 mmole), 1-[3-(4-chlorophenyl)propyl]piperazine (3.58 g; 15 mmole), triethylamine (1.52 g; 15 mmole), and ethanol (100 ml) was refluxed for 35 hours. The solvent was removed in vacuo and water added to the residue. The product was extracted with ether, dried, and concentrated in vacuo. The resulting reddish-yellow oil was purified on a silica gel column (methylene chloride/methanol 9:1) to give the product as a free base (2.8 g; 42% yield). The product was dissolved in ether and precipitated with ethereal hydrochloric acid to provide, after recrystallization from water, the title compound as colorless crystals, m.p. 219°-221° C.

1. temperaturewas refluxed for 35 hours
2. customThe solvent was removed in vacuo and water
3. additionadded to the residue
4. extractionThe product was extracted with ether
5. customdried
6. concentrationconcentrated in vacuo
7. customThe resulting reddish-yellow oil was purified on a silica gel column (methylene chloride/methanol 9:1)
8. customto give the product as a free base (2.8 g; 42% yield)
9. customprecipitated with ethereal hydrochloric acid
10. customto provide
11. customafter recrystallization from water