反应详情

A mixture of 3.12 g (13.7 mmol) of methyl 1-(2-cyanoethyl)-2-indolecarboxylate, 30 ml of 10% sodium carbonate solution, 30 ml of 30% hydrogen peroxide and 100 ml of acetone was stirred at room temperature for 4 hours. Next, the reaction mixture was cooled to 0° C. and 10% sodium sulfite solution was added dropwise to decompose an excess of the peroxide. The most of acetone in the reaction mixture was then distilled off and the concentrate was extracted three times with ethyl acetate. The combined extracts were washed with saturated sodium chloride solution. After drying over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography to give 2.30 g (68%) of methyl 1-(2-carbamoylethyl)-2-indolecarboxylate.

1. temperatureNext, the reaction mixture was cooled to 0° C.
2. distillationThe most of acetone in the reaction mixture was then distilled off
3. extractionthe concentrate was extracted three times with ethyl acetate
4. washThe combined extracts were washed with saturated sodium chloride solution
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography