反应详情

A 30% wt solution containing HBr in acetic acid (25 mL) is added to a flask containing benzyl 2-(hydroxymethyl)-5-iodo-1-indolinecarboxylate (Preparation 8, 6.03 g). All of the solids are dissolved and the solution is concentrated to give a brown solid. The crude product is taken into CH2Cl2 with a small amount of methanol and triethylamine and purified by column chromatography eluting with heptane (250 mL), 20% EtOAc in heptane (500 mL), and 40% EtOAc in heptane to give 3.92 g (84%) of the title compound as a red solid. Physical characteristics: M.p. 64-66° C.; HRMS (FAB) m/z 318.0006 (C11H12INO2+H). Anal. Found: C, 41.91; H, 3.85; N, 4.35.

1. additionis added to a flask
2. dissolutionAll of the solids are dissolved
3. concentrationthe solution is concentrated
4. customto give a brown solid
5. custompurified by column chromatography
6. washeluting with heptane (250 mL), 20% EtOAc in heptane (500 mL), and 40% EtOAc in heptane