反应详情

A mixture of 2,2-diphenyl-5-methylaminopentanamide (0.3 g--see Preparation 3), N-[4-(2-methanesulphonyloxyethyl)phenyl]-methanesulphonamide (0.3 g--see Preparation 18), sodium bicarbonate (0.5 g) and acetonitrile (10 ml) was heated under reflux for 8 hours. The mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml), the layers separated and the aqueous layer extracted with dichloromethane (2×20 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 6%). The product-containing fractions were combined and concentrated in vacuo to give the title compound as a foam, yield 0.12 g.

1. temperaturewas heated
2. temperatureunder reflux for 8 hours
3. customThe mixture was partitioned between dichloromethane (30 ml) and 10% aqueous sodium carbonate (30 ml)
4. customthe layers separated
5. extractionthe aqueous layer extracted with dichloromethane (2×20 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 6%)
11. concentrationconcentrated in vacuo