反应详情

This title compound was prepared starting from 29.B (169 mg, 0.84 mmol) and Boc-4-chloro L-phenylalanine (available from Chem-Impex International, Inc. (305 mg, 1.0 mmol) according the procedure described above for conversion of 17.B to 17.2, except that glyoxylic acid (1.0 equiv.) was used in the last step. After purification by preparative HPLC (5-40% CH3CN/water, 45 min), product fractions were collected, treated with 1.0 N HCl, and concentrated to provided 29 HCl salt as colorless solid (52 mg, 14%). MS ESI (positve.) m/e: 442.1 (M+H); 1H NMR (400 MHz, CD3OD) δ ppm 8.77 (d, J=7.04 Hz, 2H), 8.40 (d, J=7.04 Hz, 2H), 7.39-7.49 (m, 2H), 7.32-7.39 (m, 2H), 7.08 (s, 1H), 4.58 (dd, J=10.17, 5.87 Hz, 1H), 4.06 (s, 2H) 3.99 (quin, J=6.55 Hz, 1H), 3.49 (dd, J=13.30, 5.87 Hz, 1H), 3.23 (dd, J=13.30, 9.78 Hz, 1H), 2.32 (s, 1H), 1.38 (dd, J=10.96, 6.26 Hz, 6H).

1. customThis title compound was prepared
2. customAfter purification by preparative HPLC (5-40% CH3CN/water, 45 min), product fractions
3. customwere collected
4. additiontreated with 1.0 N HCl
5. concentrationconcentrated