反应详情

4-(4-(tert-butoxycarbonyl)piperazin-1-yl)-3-fluorobenzoic acid 302 (1.1 g, 3.39 mmol), propan-2-amine (0.241 g, 4.07 mmol), N1-((ethylimino)methylene)-N3,N3-dimethylpropane-1,3-diamine hydrochloride (0.975 g, 5.09 mmol) and 1H-benzo[d][1,2,3]triazol-1-ol hydrate (0.779 g, 5.09 mmol) were suspended in DMF (13.57 mL) and 4-methylmorpholine (1.864 mL, 16.96 mmol) was added. The reaction mixture was stirred at ambient temperature for 2 h, diluted with water (50 mL), and extracted with ethyl acetate (3×100 mL). The combined organic extracts were washed with brine (3×50 mL), dried over MgSO4, and concentrated in vacuo to afford the title compound as an off-white solid (1.11 g, 3.04 mmol, 89% yield). ESI-MS: m/z 366 (M+H)+.

1. extractionextracted with ethyl acetate (3×100 mL)
2. washThe combined organic extracts were washed with brine (3×50 mL)
3. dry with materialdried over MgSO4
4. concentrationconcentrated in vacuo