反应详情

ethyl 1-(1H-indole-2-carbonyl)piperidine-4-carboxylate (3.0 g, 9.99 mmol) and lithium hydroxide, H2O (4.19 g, 100 mmol)) were dissolved in THF (Ratio: 1, Volume: 20 ml) and Water (Ratio: 2, Volume: 40.0 ml) and allowed to stir overnight at room temperature. The reaction was diluted with water, and extracted with diethyl ether. The aqueous layer was acidified using 2N HCl to pH ˜2. A fine, white suspension resulted. The aqueous layer was extracted with ethyl acetate twice. The combined ethyl acetate layers were dried over magnesium sulfate, filtered and concentrated to afford the product as a white solid. (Yield: 678 mg, white solid) 1H-NMR (400 MHz, DMSO-d6) 12.33, 11.53, 7.60, 7.41, 7.21-6.94, 6.76, 4.40-4.21, 3.17, 2.66-2.53, 1.97-1.82, 1.63-1.47

1. extractionextracted with diethyl ether
2. customA fine, white suspension resulted
3. extractionThe aqueous layer was extracted with ethyl acetate twice
4. dry with materialThe combined ethyl acetate layers were dried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated