反应详情

N-Bromosuccinimide (440 mg) was added to a solution of ethyl 5-chloroindole-2-carboxylate (500 mg) in N,N-dimethylformamide (10 ml). The reaction mixture was stirred at room temperature for 18 hours, and the solvent was distilled off under reduced pressure. The residue was partitioned in ethyl acetate and water, and a water layer was extracted with ethyl acetate. The resultant organic layers were combined, washed with saturated aqueous solution of sodium chloride and then dried over anhydrous sodium sulfate. The solvent was distilled off, the residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:9), and white powder thus obtained was washed with hexane to obtain the title compound (680 mg).

1. distillationthe solvent was distilled off under reduced pressure
2. customThe residue was partitioned in ethyl acetate
3. extractionwater, and a water layer was extracted with ethyl acetate
4. washwashed with saturated aqueous solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off
7. customthe residue was purified by column chromatography on silica gel (ethyl acetate:hexane=1:9), and white powder
8. customthus obtained
9. washwas washed with hexane