Methanesulfonic Acid → HCID 54718246, compound

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Reaction Steps

To a solution of N,N-diethyl-2-hydroxy-5-chloro-β-oxo-α-(3-phenoxypropyl)benzenepropanamide (0.25 g; 6.6 mmol) (prepared in Example I) in toluene (5 ml) was added methanesulfonic acid (0.07 g; 0.7 mmol). The resulting mixture was heated to reflux and stirred for 20 minutes. The mixture was cooled and the solvent removed under reduced pressure. The residue was dissolved in a 1:1 mixture of EtOAc/Et2O (10 ml), washed with saturated aqueous NaCl, and dried (MgSO4). The solvent was removed in vacuo to provide an oil which crystallized from Et2O to provide 0.16 g (83% yield) of the title compound, m.p. 162°-163° C. NMR (DMSO-d6) δ1.90 (m, 2H), 2.68 (t, 2H), 3.99 (t, 2H), 6.91 (m, 3H), 7.26 (m, 2H), 7.41 (d, 1H), 7.63 (dd, 1H), 7.95 (d, 1H).

Provenance & Evidence