Methanesulfonic Acid → HCID 11606046, compound

Participants

Reaction Steps

A solution of methane sulfonic acid (0.058 mL, 0.852 mmol) in methanol (1 mL) was added to a solution of compound of Example 18 (0.3 g, 0.710 mmol) in methanol (10 mL) at 25° C. and filtered. The solution was stirred for 1 h and the precipitated solid was filtered, washed using methanol and dried to obtain the title compound. Yield: 0.244 g, (66%); mp 278-280° C.; 1H NMR (DMSO-d6, 300 MHz): δ 2.31 (s, 3H, CH3), 2.62 (s, 3H, CH3), 3.21 (s, 4H, 2CH2), 3.38 (s, 4H, 2CH2), 5.16 (s, 2H, CH2), 7.19 (s, 1H, Ar), 7.19 (s, 1H, Ar), 8.06 (s, 1H, Ar), 8.13 (s, 1H, Ar), 8.80 (s, 1H, NH); MS: m/e (ES+) 423 (M+1, freebase); analysis: C20H23ClN2O8S2 requires C, 46.29; H, 4.47; N, 5.40; Cl, 6.83; S, 12.36. found: C, 46.75; H, 4.26; N, 5.37; Cl, 7.33; S, 12.58%.

Provenance & Evidence