反应详情

1-(1-(4-chlorobenzyl)-1H-indole-2-carbonyl)piperidine-4-carboxylic acid (100 mg, 0.252 mmol), N1-((ethylimino)methylene)-N3,N3-dimethylpropane-1,3-diamine hydrochloride (72.5 mg, 0.378 mmol), and 1H-benzo[d][1,2,3]triazol-1-ol (51.1 mg, 0.378 mmol) were dissolved in DCM (Volume: 3.0 mL). The reaction was stirred for 10 minutes before 2-(4-chlorophenyl)ethanamine (0.053 mL, 0.378 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.066 mL, 0.378 mmol). The reaction was stirred overnight at room temperature. The reaction was diluted with water and ethyl acetate. The organic layer was washed with 1N HCl, saturated sodium bicarbonate solution, and finally saturated sodium chloride. the organic layer was then dried over magnesium sulfate, filtered and concentrated. The crude material was triturated in ethyl acetate to give the product as a white solid. (Yield: 60 mg, white solid) 1H-NMR (400 MHz, DMSO-d6) 7.85, 7.63, 7.54, 7.38-7.31, 7.24-7.18, 7.14-7.06, 6.71, 5.49, 4.37, 4.00, 3.26, 2.92, 2.69, 2.37-2.27, 1.76-1.22

1. washThe organic layer was washed with 1N HCl, saturated sodium bicarbonate solution, and finally saturated sodium chloride
2. dry with materialthe organic layer was then dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude material was triturated in ethyl acetate