反应详情

The solution obtained in step 1 was cooled to 4-5° C. in an ice bath, followed by dropwise adding triethylamine (0.42 ml, 3.0 mmol) for 5 min. To the reaction solution was added with 4-(4-fluorobenzyl)morpholin-2-ylmethylamine (1.2 mmol), and stirred for 30 min at a room temperature and then for an additional 4 hrs under reflux. The reaction mixture was cooled to a room temperature, and washed with saturated aqueous sodium hydrogen carbonate solution and then with saturated saline. After water was removed with a desiccant, the resulting solution was concentrated in a reduced pressure. In order to obtain a desired fraction, the residue was subjected to silica column chromatography (mobile phase: 30 (v/v) % Hexane in EA) to afford the title compound (Total yield: 53.0%)1H NMR (CDCl3) δ 8.20 (d, 1H), 8.12 (d, 1H), 7.54 (d, 1H), 7.36-7.24 (m, 7H), 7.01 (t, 2H), 6.46-6.38 (m, 1H), 4.08-3.98 (m, 1H), 3.87 (d, 1H), 3.73-3.61 (m, 4H), 3.53 (s, 2H), 3.45 (s, 2H), 3.32-3.19 (m, 2H), 2.85-2.61 (m, 4H), 2.32-2.14 (m, 3H), 2.08-1.88 (m, 3H) ppm.

1. temperaturefor an additional 4 hrs under reflux
2. temperatureThe reaction mixture was cooled to a room temperature
3. washwashed with saturated aqueous sodium hydrogen carbonate solution
4. customAfter water was removed with a desiccant, the resulting solution
5. concentrationwas concentrated in a reduced pressure
6. customIn order to obtain a desired fraction