Hydrochloric Acid → HCID 57925981, compound

Participants

Reaction Conditions

Reaction Steps

To a solution [4-(2-tert-butoxycarbonylamino-5-thiophen-2-yl-phenylcarbamoyl)-benzyl]-methyl-phosphinic acid ethyl ester (377 mg, 0.733 mmol) in dioxane (2 mL) was added NaOH (1 mL, 5.00 mmol, 5M) and the solution was heated to 60° C. After 18 h, the reaction was diluted with EtOAc, acidified with 1N HCl. The organic layer was dried (MgSO4), filtered and the solvent was evaporated under reduced pressure. The material was used without further purification. 1H NMR (DMSO-d6) δ 9.94 (s, 1H), 8.74 (br s, 1H), 7.91 (d, J=8.2 Hz, 2H), 7.79 (d, J=2.0 Hz, 1H), 7.58 (d, J=8.5 Hz, 1H), 7.50 (dd, J=5.0, 1.2 Hz, 1H), 7.48 (dd, J=8.5, 2.0 Hz, 1H), 7.44-7.39 (m, 3H), 7.10 (dd, J=5.3, 3.5 Hz, 1H), 3.13 (d, J=17.9 Hz, 2H), 1.43 (s, 9H), 1.21 (d, J=13.8 Hz, 3H). MS: cal'd 387 (MH+; -Boc), exp 387 (MH+; -Boc).

Provenance & Evidence