Trifluoroacetic acid → HCID 70800861, compound

Participants

Reaction Steps

To a solution of Compound 46a (1.16 g, 2.3 mmol) in DCM (10 mL) was added TFA (5 mL) and the reaction mixture stirred for 0.5 h. The reaction mixture was concentrated under reduced pressure then evaporated under reduced pressure from toluene (2×). The residue was diluted with 1.5 M K3PO4 then extracted with DCM (3×). The combined extracts were washed with brine, dried (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by silica gel chromatography eluting with 1 to 15% MeOH/DCM to give Compound 46b (68 mg, 74% yield) as a pale brown solid. LCMS=1.71 min using analytical method (B), 402.0 (M+H). 1H NMR (400 MHz, CD3OD) δ 8.24 (d, J=1.5 Hz, 1H), 8.01 (d, J=8.8 Hz, 1H), 7.79 (dd, J=8.5, 1.8 Hz, 1H), 7.73-7.65 (m, 2H), 7.47 (t, J=7.7 Hz, 2H), 7.41-7.32 (m, 1H), 4.47 (s, 2H).

Provenance & Evidence