Trifluoroacetic acid → HCID 25013303, compound

Participants

Reaction Steps

To a solution of [4-(2-tert-butoxycarbonylamino-5-thiophen-2-yl-phenylcarbamoyl)-benzyl]-methyl-phosphinic acid ethyl ester (500 mg, 0.972 mmol) in DCM (10 mL) was added TFA (5 mL, 64.9 mmol). After 2 h, the solvent was removed, and to the residue was added EtOAc and sat. NaHCO3. The aqueous fraction was extracted further with EtOAc, dried (MgSO4), filtered and the solvent was evaporated under reduced pressure. The material was used without further purification. 1H NMR (DMSO-d6) δ 9.69 (br s, 1H), 7.92 (d, J=7.9 Hz, 2H), 7.44 (m, 1H), 7.39 (dd, J=7.9, 2.0 Hz, 1H), 7.33 (dd, J=5.0, 1.8 Hz, 1H), 7.27 (dd, J=8.2, 2.0 Hz, 1H), 7.21 (dd, J=3.5, 1.0 Hz, 1H), 7.02 (dd, J=5.0, 3.5 Hz, 1H), 6.78 (d, J=8.2 Hz, 1H), 5.13 (s, 2H), 3.97-3.88 (m, 2H), 3.40-3.25 (m, 2H), 1.32 (d, J=13.8 Hz, 3H), 1.27 (t, J=7.0 Hz, 3H). MS: cal'd 415 (MH+), exp 415 (MH+).

Provenance & Evidence