反应详情

The reaction mixture (now a heterogeneous paste) was poured into a mechanically-stirred slurry of ice water (1:1, 1L), the precipitate filtered and bashed with water (2×100 ml), saturated aqueous sodium bicarbonate (4×200 ml) and finally water to neutral pH (4×300 ml). The product was dried overnight at 40° C. and 0.3 mm Hg over KOH pellet, then redried over P2O5 to yield 5-(N-methyl acetamido)-2,4,6-triiodoisophthaloyl dichloride (XIV) as a slightly off-white, granular solid (60.0 g, 92% yield). TLC (85% CCl4 /15% acetone): Rf (XII):0.79; Rf (XIV):0.59.