Trifluoroacetic acid → HCID 70800861, compound

Participants

Reaction Steps

To a solution of Compound 24a (1.16 g, 2.30 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 azeotroped from toluene (2×). The crude residue was diluted with 1.5M K3PO4 then the aqueous layer extracted with DCM (3×). The combined organic extracts were washed with brine, dried (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified on silica gel eluting with 0-15% MeOH/DCM to give Compound 24b (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