反应详情

To a solution of 1-(2-aminoethyl)-6-methoxyindan (1.00 g, 5.23 mmol), 1-benzyloxycarbonyl-4-piperidinecarboxylic acid (1.38 g, 5.23 mmol) and 1-hydroxy-1H-benzotriazole (0.78 g, 5.75 mmol) in DMF (20 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (WSC; 1.10 g, 5.75 mmol). The mixture was stirred for 6 hours at room temperature. To the reaction mixture was added water, and the mixture was subjected to extraction with ethyl acetate. The extract solution was washed with brine, which was dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. The residue was purified by means of a silica gel column chromatography (chloroform/methanol, 95:5) to give 2.10 g (yield 92%) of the above-titled compound, m.p.132-133° C. (recrystallized from ethyl acetate/isopropyl ether).

1. extractionthe mixture was subjected to extraction with ethyl acetate
2. washThe extract solution was washed with brine, which
3. dry with materialwas dried over anhydrous magnesium sulfate
4. distillationby distilling off the solvent under reduced pressure
5. customThe residue was purified by means of a silica gel column chromatography (chloroform/methanol, 95:5)
6. customto give