Reaktion #11205

ord-6204db7a9e304c63b085f7c35e35f930

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Vorschrift

Demethylation of (116) prepared as described in example 229 with pyridinium hydrochloride using the procedure described in example 81 gave (117) (50%) as a yellow powder, mp 286° C. 1H NMR δ [(CD3)2SO] 12.40 (br, 1H), 11.06 (br s, 1H), 9.37 (br s, 1H), 8.37 (d, J=2.4 Hz, 1H), 7.81 (s, 1H), 7.59 (d, J=8.7 Hz, 1H), 7.57 (m, 1H), 7.53–7.43 (m, 3H), 7.13 (dd, J=8.7, 2.4 Hz, 1H), 4.67 (t, J=6.8 Hz, 2H), 2.74 (t, J=6.8 Hz, 2H). Found: C, 60.00; H, 3.65; N, 5.52. C23H15ClN2O5.1.5H2O requires C, 59.81; H, 3.92; N, 6.06.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094798B1uspto-grants-2006_08