Chlorosulfamic acid → HCID 68493881, compound

Participants

Reaction Steps

Sulfamoylation of 226 with H2NSO2Cl and DMA as described above afforded the title compound (86 mg, 89%) as a colourless foam. 1H NMR (400 MHz; DMSO-d6) 1.14 (6H, s, 2×CH3), 2.69 (2H, s, CH2), 3.43 (2H, s, CH2), 3.62 (2H, s, CH2), 3.73 (3H, s, OCH3), 3.75 (3H, s, OCH3), 6.80 (1H, dd, J=8.0, 2.0 Hz, CH), 6.83 (1H, s, CH), 6.89-6.94 (3H, m, 3×CH), 7.23 (1H, t, J=8.0 Hz, CH), 7.79 (2H, s, NH2). 13C NMR (100 MHz; DMSO-d6) 42.80 (CH2), 49.42 (CH2), 52.05 (C), 53.0 (CH2), 54.94 (OCH3), 55.79 (OCH3), 111.83 (CH), 112.97 (CH), 114.10 (CH), 120.30 (CH), 120.61 (CH), 125.77 (C), 129.25 (CH), 133.04 (C), 136.80 (C), 142.19 (C), 149.88 (C), 159.28 (C). LC/MS (ES+) tr=1.14 min, m/z 407.28 (M++H). HRMS (ES+) cald. for C20H27N2O5S (M++H) 407.1635, found 407.1636. HPLC tr=2.10 min (>98%).

Provenance & Evidence