反应详情

A solution of 1-(3,4-dichlorobenzyl)-piperidin-4-ylamine (2.2 g; JP 59101483) and triethylamine (1.53 ml) in dichloromethane (100 ml) stirring at ambient temperature was treated with 3-chlorocarbonyl-propionic acid methyl ester (1.14 ml). After stirring for 16 hours, the reaction mixture was washed with brine, the organic layer was dried (MgSO4), and evaporated to leave a white solid. This solid was suspended in ethanol (100 ml), treated with hydrazine hydrate (5 ml) and the resulting mixture was stirred at reflux for 2 hours and then allowed to cool. Water (30 ml) was added to the reaction mixture and the ethanol was evaporated. The aqueous residue was then extracted into dichloromethane (6×50 ml), the combined organics were dried (MgSO4) and evaporated to give the subtitle compound as a white solid. (1.9 g)

1. washthe reaction mixture was washed with brine
2. dry with materialthe organic layer was dried (MgSO4)
3. customevaporated
4. customto leave a white solid
5. stirringthe resulting mixture was stirred
6. temperatureat reflux for 2 hours
7. temperatureto cool
8. customthe ethanol was evaporated
9. extractionThe aqueous residue was then extracted into dichloromethane (6×50 ml)
10. dry with materialthe combined organics were dried (MgSO4)
11. customevaporated