反应详情

68.2 g (118.6 mmol) of 1,4,7-tris-(benzyloxycarbonyl)-1,4,7,10-tetrazacyclododecane (Delaney et al., J Chem. Soc. Perkin Trans. 1991, 3329) is dissolved in 700 ml of acetonitrile and mixed with 75.4 g (545.5 mmol) of sodium carbonate. Then, 39.6 g (355.5 mmol) of bromoacetic acid ethyl ester is added while being stirred vigorously, and it is heated for 20 hours to 40° C. Insoluble components are filtered out, evaporated to the dry state and chromatographed on silica gel (mobile solvent: ethyl acetate/hexane 20:1). The fractions that contain the product are combined and concentrated by evaporation.

1. temperatureit is heated for 20 hours to 40° C
2. filtrationInsoluble components are filtered out
3. customevaporated to the dry state
4. customchromatographed on silica gel (mobile solvent: ethyl acetate/hexane 20:1)
5. concentrationconcentrated by evaporation