Acetate → HCID 59824358, compound

Participants

Reaction Steps

In dry three necked round bottom flask fitted with an additional funnel was poured 5 amino 2, 4, 6 triiodo isophthalic 3 ally amide (7) (10 g, 0.016 mol) and 10 ml of DMAC. To the stirred and cooled solution 1, 3 acetate 4 carbonyl chloride 2, 2 dimethyl (15) (6.8 g, 0.032 mol) in 10 ml of DMAc was added dropwise over 15-20 minutes. The reaction was allowed to react 20 hours with a gentle flow of nitrogen bubbling through the reaction. The solvent was concentrated under vacuo and the resulting dark brown crude mixture was purified via normal phase column chromatography eluting with ethyl acetate and petroleum ether. After purification 11 g of an off-white solid was obtained (90% yield and 98% HPLC purity)

Provenance & Evidence