反应详情

A solution of the product from Step 5 (13.9 g, 33.4 mmol) in EtOAc (700 mL) was cooled in an ice bath and saturated with hydrogen chloride gas. The reaction flask was sealed and allowed to warm to RT. After 3.5 hours, the solvent was removed by evaporation to give the title compound as a gray solid, 11.2 g. 1H NMR (500 MHz, ppm, CD3OD) δ 7.47-7.45 (m, 1H), 7.32-7.31 (m, 1H), 7.26-7.21 (m, 1H), 6.79-6.73 (m, 1H), 5.79-5.73 (m, 1H), 5.46 (s, 1H), 5.41-5.38 (m, 1H), 4.80-4.72 (m, 4H), 3.91 (s, 3H), 3.74-3.63 (m, 2H), 2.77-2.71 (m, 1H), 2.51-2.46 (m, 1H). LRMS (ESI) m/z 317 [(M+H)+; calcd for C17H21N2O4: 317].

1. customThe reaction flask was sealed
2. customthe solvent was removed by evaporation