Methanesulfonic Acid → HCID 11541071, compound

Participants

Reaction Steps

A solution of methane sulfonic acid (0.023 mL, 0.3612 mmol) in methanol (1 mL) was added to a solution of 4-chloro-6-methyl-10,10-dioxo-2-piperazin-1-yl-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid methyl ester (free base of example 16, 0.15 g, 0.344 mmol) in methanol (10 mL) at 25° C. and stirred for 15 min. The resultant precipitate was filtered, washed using methanol and dried to obtain the title compound. Yield: 0.13 g, (71%); mp 279-281° C.; 1H NMR (CDCl3, 300 MHz): δ 2.30 (s, 3H, CH3), 2.63 (s, 3H, CH3), 3.22 (s, 4H, 2CH2), 3.39 (s, 4H, 2CH2), 3.85 (s, 3H, OCH3), 5.17 (s, 2H, CH2), 7.18 (s, 1H, Ar), 7.20 (s, 1H, Ar), 8.09 (s, 1H, Ar), 8.15 (s, 1H, Ar), 8.72 (s, 2H, NH2); MS: m/e (ES+) 437 (M+1, free base); analysis: C21H25ClN2O8S2 requires C, 47.32,H, 4.73, N, 5.26, Cl, 6.65, S, 12.03; found: C, 47.80, H, 4.93, N, 5.44, Cl, 7.07, S, 11.75%.

Provenance & Evidence