Triethyl phosphite → HCID 87849905, compound

Participants

Reaction Steps

A solution of compound 4 (0.08 g, 0.16 mmol) in 10 mL of (EtO)3P was stirred at 140° C. for 24 h and the solvent was evaporated under reduced pressure. The residue was dissolved in 10 mL of MeOH and adsorbed on silica gel and then purified on silica gel column chromatography (Hexane:EtOAc=1:2 to 1:4 v/v) to give compound 5 (0.04 g, 0.07 mmol) in 44% yield. 1H NMR (CDCl3, 400 MHz) δ 8.97 (br, 1H), 8.08 (d, J=7.2, 2H), 8.04 (d, J=7.6, 1H), 7.92 (d, J=7.2, 2H), 7.60 (m, 3H), 7.50 (m, 4H), 5.98 (d, J=18.4, 1H), 5.65 (d, J=4.8, 0.5H), 5.52 (d, J=4.8, 0.5H), 5.45 (m, 1H), 4.76 (m, 1H), 4.11 (m, 4H), 2.42 (m, 2H), 1.32 (m, 6H); MS calcd for C27H29FN3O8P m/z 574.2 (M+H)+, found 574.3.

Provenance & Evidence