反应详情

In a 1 l flask, 23.5 g of ethyl 6-cyanoindole-2-carboxylate was dissolved in 300 ml of dimethylformamide, and 6.6 g of 60% NaH was slowly added thereto at 0° C. 17.6 ml of iodoethane was then added thereto at −10˜0° C. and the mixture was stirred for 2 hours at room temperature. The reaction solution was cooled and, after adding ice, diluted with water and then extracted three times with ethyl acetate. The organic extracts were combined, dried over MgSO4 and then evaporated. The residue was purified with silica gel column chromatography [eluent: ethyl acetate/n-hexane(1:3)]. The fractions containing the desired product were combined and then evaporated to obtain 26.2 g of the title compound as a yellow solid.

1. customat 0° C
2. temperatureThe reaction solution was cooled
3. additionafter adding ice
4. extractionextracted three times with ethyl acetate
5. dry with materialdried over MgSO4
6. customevaporated
7. customThe residue was purified with silica gel column chromatography [eluent: ethyl acetate/n-hexane(1:3)]
8. additionThe fractions containing the desired product
9. customevaporated