反应详情

To a stirred solution of sodium diatrizoate (7.1 g, 11.2 mmol) in dry dimethylformamide (50 ml) at room temperature under a blanket of argon was added a solution of diethyl 2-bromoethylphosphonate (3.02 g, 12.3 mmol, 1.1 eq.) in dimethylformamide (10 ml). After stirring for 12 hours, the solvent was evaporated under vacuum to give a white solid that was washed with 300 ml of saturated aqueous NaHCO3, and then extracted with a 2:1 mixture of chloroform-ethanol (3×200 ml). The organic extract was dried (MgSO4), filtered, and evaporated under vacuum to give 3.61 g (41%) of product as a white solid. Recrystallization from acetonitrile gave analytically pure material; mp 249-251° C.; MH+ (779). The 1H-NMR (300 MHz) spectrum was consistent with the desired material.

1. customthe solvent was evaporated under vacuum
2. customto give a white solid
3. washthat was washed with 300 ml of saturated aqueous NaHCO3
4. extractionextracted with a 2:1 mixture of chloroform-ethanol (3×200 ml)
5. extractionThe organic extract
6. dry with materialwas dried (MgSO4)
7. filtrationfiltered
8. customevaporated under vacuum