反应详情

2.36 g of ethyl N-(2,4-dichloro-1,3,5-triazin-6-yl)-glycinate [obtained as described in Preparation 4(A)], 4.19 g of 2,2,6,6-tetramethyl-4-(butylamino)piperidine [obtained as described in Preparation I(A)] and 2.77 g of sodium bicarbonate were heated under reflux in 20 ml of xylene for 29 hours. At the end of this time, the xylene was removed by distillation under reduced pressure, and a mixture of methylene chloride and water was added to the resulting residue, after which the mixture was shaken. The methylene chloride layer was separated, dried and concentrated by evaporation under reduced pressure, and the resulting residue was purified by silica gel column chromatography (using a 20:10:1:1 by volume mixture of hexane, diethyl ether, ethanol and triethylamine as eluent), to yield 5.46 g of the title compound melting at40° C.

1. customAt the end of this time, the xylene was removed by distillation under reduced pressure
2. additiona mixture of methylene chloride and water
3. additionwas added to the resulting residue
4. customThe methylene chloride layer was separated
5. customdried
6. concentrationconcentrated by evaporation under reduced pressure
7. customthe resulting residue was purified by silica gel column chromatography (
8. additionby volume mixture of hexane, diethyl ether, ethanol and triethylamine as eluent),