Hydrochloric Acid → HCID 9811363, compound

Participants

Reaction Steps

A solution of bis-(4-hydroxy-3,5-diiodophenyl)-methanone (prepared according to Example 9, 3.59 g, 5.0 mmol) and benzyl 2-bromoacetate (1.15 g, 5.0 mmol) in 20 mL DMAc was stirred with cesium carbonate (3.3 g, 10 mmol) for 14 hours. Next was added 1 M HCl, and a yellow oil formed along with a hazy white precipitate. The precipitate was isolated by filtration and was recrystallized from hot isopropanol/chloroform, yielding the title compound as colorless crystals (98 mg, 2.2%). No attempt was made to isolate more product from the oil. 1H NMR (400 MHz, CDCl3): δ 8.11 (s, 2H), 8.10 (s, 2H), 7.45-7.35 (m, 5H), 6.22 (s, 1H), 5.33 (s, 2H), 4.72 (s, 2H). HPLC (40-90), 19.17 min. (EI−) calc'd for [C22H14I4O5—H] 864.7, found 864.6.

Provenance & Evidence