反应详情

A mixture containing 2,2-diphenyl-5-methylaminopentanamide (0.36 g--see Preparation 1), 6-(2-bromoethyl)-1,4-benzodioxan (0.32 g), anhydrous potassium carbonate (0.75 g) and acetonitrile (20 ml) was heated under reflux for 16 hours. The mixture was partitioned between dichloromethane (50 ml) and 10% aqueous sodium carbonate (30 ml), the layers separated and the aqueous layer extracted with dichloromethane (3×20 ml). The combined dichloromethane extracts were dried (MgSO4) and concentrated in vacuo to give an oil which was purified by column chromatography on silica eluting with dichloromethane containing methanol (0% up to 5%). The product-containing fractions were combined and concentrated in vacuo to give a foam which was further purified by column chromatography on alumina eluting with dichloromethane containing methanol (0% up to 5%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a foam, yield 0.11 g.

1. temperaturewas heated
2. temperatureunder reflux for 16 hours
3. customThe mixture was partitioned between dichloromethane (50 ml) and 10% aqueous sodium carbonate (30 ml)
4. customthe layers separated
5. extractionthe aqueous layer extracted with dichloromethane (3×20 ml)
6. dry with materialThe combined dichloromethane extracts were dried (MgSO4)
7. concentrationconcentrated in vacuo
8. customto give an oil which
9. customwas purified by column chromatography on silica eluting with dichloromethane
10. additioncontaining methanol (0% up to 5%)
11. concentrationconcentrated in vacuo
12. customto give a foam which
13. customwas further purified by column chromatography on alumina eluting with dichloromethane
14. additioncontaining methanol (0% up to 5%)
15. concentrationconcentrated in vacuo