反应详情

A mixture of 5-hydroxy-1-(2,2,2-trifluoro-ethyl)-1H-indole-2-carboxylic acid (intermediate 1, step c, 7.62 g, 1.0 eq.), 2-(1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (12.8 g, 1.3 eq.), morpholine (3.36 mL, 1.3 eq.) and N-ethyldiisopropylamine (25.7 mL, 5 eq.) in dimethylformamide (85 mL) was stirred at room temperature for 24 h. The reaction mixture was diluted with ethyl acetate and washed with hydrochloric acid (1N), water and brine and dried over sodium sulfate, filtered and concentrated in vacuo. The precipitate was filtered, washed with ethyl acetate and dried in vacuo to yield 7.15 g (74%) of the desired product as off-white solid. MS (m/e): 329.5 (MH+, 100%).

1. washwashed with hydrochloric acid (1N), water and brine
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. filtrationThe precipitate was filtered
6. washwashed with ethyl acetate
7. customdried in vacuo