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To 500 mL of dry N,N-dimethylformamide was added 159 g (0.250 mol) sodium diatrizoate and 54.5 g (0.280 mol) of ethyl 2-bromobutyrate. The mixture was heated on a steam bath for 20 h, cooled to room temperature and poured into 3 L of dilute ammonium hydroxide. The solid was filtered, washing with water, and air-dried. The solid was further purified by crystallization from 50% aqueous ethanol (after treatment with decolorizing carbon) affording two crops which were dried at 100° C. overnight to afford 121 g (66%) of a white powder, m.p. 288°-290° C. (dec.). Analysis for C17H19I3N2O6 : Calculated/Found: C, 28.05/28.36/H, 2.63/2.55; I, 52.3/52.3.

1. temperatureThe mixture was heated on a steam bath for 20 h
2. filtrationThe solid was filtered
3. washwashing with water
4. customair-dried
5. customThe solid was further purified by crystallization from 50% aqueous ethanol (after treatment with decolorizing carbon)
6. customaffording two crops which
7. customwere dried at 100° C. overnight