4-(Chlorosulfonyl)-2-hydroxybenzoic acid → HCID 9874697, compound

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Reaction Steps

The title compound was prepared according to the procedure in Example 4 using (4-hydroxy-3,5-diiodo-phenyl)-(4-methoxy-phenyl)-methanone (0.202 g, 0.421 mmol) and 4-chlorosulphonyl-2-hydroxybenzoic acid (0.398 g, 1.68 mmol) in THF (5 mL). Purification by preparative HPLC (C18, eluting with 70% CH3CN/H2O containing 0.1% TFA) gave 0.045 g (16%) of the title compound as a white solid, mp 214-215° C. 1H NMR (DMSO-d6) δ 3.86 (s, 3H), 7.11 (d, 2H), 7.44-7.48 (m, 2H), 7.73 (d, 2 H), 8.04-8.07 (m, 3H). IR (KBr) 3400, 3050, 1690, 1600, 1260 and 1175 cm-1. mass spectrum (-ESI) m/z 679 (M-H). Anal. Calcd. for C21H14I2O8S: C,37.08; H,2.07; N,0.00. Found: C,37.43; H,2.24; N,0.00.

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