反应详情

Anhydrous DMF solution (10 ml) of 2-t-butoxycarbonyl-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole (2.72 g, 10 mol) was mixed with 60% sodium hydride (0.4 g, 10 mmol) and stirred at room temperature for 1 hour. The reaction solution was cooled to −60° C., mixed with 2-acetoxy-1-bromoethane (1.67 g, 10 mmol) and then returned to room temperature while stirring for 1 hour. The reaction solution was mixed with ethyl acetate, washed with water and dried with anhydrous sodium sulfate, and then the solvent was removed by evaporation under a reduced pressure, the thus obtained residue was mixed with diisopropyl ether (20 ml) and the thus precipitated crystals were collected by filtration to obtain 1.90 g of the title compound (5.3 mmol, 53% in yield).

1. temperatureThe reaction solution was cooled to −60° C.
2. customreturned to room temperature
3. stirringwhile stirring for 1 hour
4. washwashed with water
5. dry with materialdried with anhydrous sodium sulfate
6. customthe solvent was removed by evaporation under a reduced pressure
7. additionthe thus obtained residue was mixed with diisopropyl ether (20 ml)
8. filtrationthe thus precipitated crystals were collected by filtration