反应详情

The title compound was prepared according to the procedure in Example 4 using commercial 4-hydroxy-4'methoxybenzophenone (0.206 g, 0.903 mmol) and 4-chlorosulphonyl-2-hydroxybenzoic acid (0.427 g, 1.81 mmol) in THF (5 mL). Purification by preparative HPLC (C18, eluting with 60% CH3CN/H2O containing 0.1% TFA) and crystallization from EtOAc/hexane gave 0.21 g (54%) of the title compound as an off white solid, mp 73-75° C.; 1H NMR (DMSO-d6) δ 3.85 (s, 3H), 7.07 (d, 2H), 7.24 (d, 2H), 7.36-7.38 (m, 2H), 7.68-7.73 (m, 4H), 7.99 (s, 1 H). IR (KBr) 3400, 1700, 1650, 1000 and 1260 cm-1. mass spectrum (-ESI) m/z 427 (M-H).

1. customThe title compound was prepared
2. customPurification
3. washby preparative HPLC (C18, eluting with 60% CH3CN/H2O containing 0.1% TFA) and crystallization from EtOAc/hexane