Chlorosulfamic acid → HCID 59380384, compound

Participants

Reaction Steps

To a solution of 2-(4-{[3-chloro-4-(pyridin-2-ylmethoxy)phenyl]amino}[1]benzothieno[2,3-d]pyrimidin-7-yl)ethanol (35 mg, 0.08 mmol, 1 equiv) in N,N-Dimethylacetamide (2 mL) was added chlorosulfonamide (87 mg, 0.76 mmol, 10 equiv) under nitrogen. The reaction mixture was stirred at rt for 15 h. The solvent was concentrated in vacuo. The crude material was separated by pre-HPLC to give a white solid (18.6 mg, 43%) as product. 1H-NMR (DMSO-d6) δ 9.0 (broad s, 1H), 8.60 (d, J=4.6 Hz, 1H), 8.54 (s, 1H), 8.53 (d, J=8.5 Hz, 1H), 8.03 (s, 1H), 7.88 (t, 1H), 7.77 (d, J=2.2 Hz, 1H), 7.59 (d, J=7.8 Hz, 1H), 7.54 (m, 2H), 7.37 (t, 1H), 7.26 (d, J=8.7 Hz, 1H), 5.32 (s, 2H), 4.36 (t, 2H), 3.19 (t, 2H); LCMS RT=3.08 min, [M+H]+=542.10

Provenance & Evidence