反应详情

A solution of 2-aminoethyl nicotinate dihydrochloride (1.25 g, 52 mmol) and 2,4,5-trichlorophenyl-N-(2-chloroethyl)-N-nitrosocarbamate (2 g, 6 mmol) in 40 mL of pyridine was stirred under nitrogen at room temperature for 24 hours. The reaction was monitored by thin layer chromatography (silica, 1:1 chloroform/ethyl acetate, Rf 0.26). The solvent was removed in vacuo and the residue was chromatographed on a silica gel column by eluting, first with benzene to remove unreacted nitrosocarbamate and trichlorophenol by-product, and then with chloroform, to qive the desired product. The resultant oil solidified in the freezer. It melted at 63°-64° C. and had the formula ##STR151##

1. customThe solvent was removed in vacuo
2. customthe residue was chromatographed on a silica gel column
3. washby eluting, first with benzene
4. customto remove unreacted nitrosocarbamate and trichlorophenol by-product