反应详情

6 g of 1-(4-aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]-piperazine (see EP-A-489 690, Example 3), 2.4 g of 2-bromoethanol and 0.6 g of 4-dimethylaminopyridine are suspended in 80 ml of isopropanol and boiled at reflux for 22 hours, then concentrated by evaporation and partitioned between methylene chloride and 1N sodium hydroxide solution. The organic phase is washed with water, dried and concentrated by evaporation. The oily material is chromatographed over 150 g of silica gel. Elution with methylene chloride/methanol (100:4 and 100:5) yields 1-[4-N-(2-hydroxyethyl)-amino]-benzoyl]-4-[2-(4-chlorophenyl)-ethyl]-piperazine, m.p. 94°-95°.

1. temperatureat reflux for 22 hours
2. concentrationconcentrated by evaporation
3. custompartitioned between methylene chloride and 1N sodium hydroxide solution
4. washThe organic phase is washed with water
5. customdried
6. concentrationconcentrated by evaporation
7. customThe oily material is chromatographed over 150 g of silica gel
8. washElution with methylene chloride/methanol (100:4 and 100:5)