反应详情

温度

0 °C

To a stirred solution of methyl 2-propylindole-6-carboxylate (911 mg) in acetonitrile (15 ml) was added chlorosulfonylisocyanate (0.6 g) in acetonitrile (1.5 ml) at 0° C. The mixture was stirred at 0° C. for 30 minutes, then N,N-dimethylformamide (0.35 g) in acetonitrile (15 ml) was added at 0° C. The resultant mixture was stirred at 20° C. for 40 minutes, and then poured into water. The mixture was extracted with methylene chloride three times, and the combined organic phase was dried over sodium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel eluting with a mixture of ethyl acetate and hexane (1:3) to give the crystals which were recrystallized from a mixture or ethyl acetate and hexane to give methyl 3-cyano-2-propylindole-6-carboxylate (535 mg) as colorless crystals.

1. extractionThe mixture was extracted with methylene chloride three times
2. dry with materialthe combined organic phase was dried over sodium sulfate
3. customevaporated in vacuo
4. customThe residue was chromatographed on silica gel eluting with a mixture of ethyl acetate and hexane (1:3)
5. customto give the crystals which
6. customwere recrystallized from a mixture or ethyl acetate and hexane