反应详情

温度

120 °C

A solution of Example 129D (0.1112 g, 0.303 mmol) in 4:1 THF/H2O in a Parr bomb was treated with triethylamine (92 μL) and PdCl2(dppf) (24.8 mg). The bomb was charged to 700 psi with CO, stirred for 24 hours at 120° C., and concentrated. The concentrate was purified by C18 reverse-phase HPLC using acetonitrile/water/0.1% TFA to provide the desired product. MS (ESI(+)) m/e 332 (M+H)+, 349 (M+NH4)+, 354 (M+Na)+; MS (ESI(−)) m/e 330 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 7.72 (m, 1H), 7.52 (m, 4H), 7.33 (d, 1H), 7.22 (d, 1H), 2.99 (m, 1H), 2.88 (m, 1H), 2.73 (m, 1H), 2.27 (m, 1H).

1. additionThe bomb was charged to 700 psi with CO
2. concentrationconcentrated
3. customThe concentrate was purified by C18 reverse-phase