反应详情

温度

-20 °C

A 20 ml portion of 1,2-dichloroethane solution containing 0.50 g (1.62 mmol) of 2a-(4-bromobutyl)-2a,3,4,5-tetrahydrobenz[cd]-indole-2(1H)-one was cooled to −20° C. and mixed with 0.10 ml (1.94 mmol) of bromine. The reaction solution was stirred at −20° C. for 1 hour, extracted with chloroform and then washed with saturated sodium thiosulfate aqueous solution and saturated sodium bicarbonate aqueous solution in that order. After drying (Na2SO4), the solvent was evaporated under a reduced pressure, and the thus obtained residue was re-precipitated from ethyl acetate-hexane to obtain 0.54 g of the title compound (86% in yield).

1. extractionextracted with chloroform
2. washwashed with saturated sodium thiosulfate aqueous solution and saturated sodium bicarbonate aqueous solution in that order
3. dry with materialAfter drying (Na2SO4)
4. customthe solvent was evaporated under a reduced pressure
5. customthe thus obtained residue was re-precipitated from ethyl acetate-hexane