反应详情

A mixture of 5.00 g (21.5 mmol) 4-chloro-6-nitro-3-quinolinecarbonitrile, 200 ml ethanol, and 3.40 g (25.8 mmol) 5-aminoindole was heated to reflux under N2 for 3.5 hours. Removed heat, made basic with saturated sodium bicarbonate and stripped solvents, azeotroping with ethanol. Collected solids and washed with hexane, then water. Dissolved solids in 200 ml ethyl acetate, added Darco and filtered. Stripped solvent and dried in vacuo overnight (50° C.). Washed twice more with ether to removed starting material aminoindole. 4.372 g of red-brown solid: mass spectrum (m/e electrospray): M+H=330.2.

1. temperaturewas heated
2. temperatureto reflux under N2 for 3.5 hours
3. customRemoved
4. temperatureheat
5. customazeotroping with ethanol
6. customCollected solids
7. washwashed with hexane
8. dissolutionDissolved solids in 200 ml ethyl acetate
9. additionadded Darco
10. filtrationfiltered
11. customStripped solvent and dried in vacuo overnight (50° C.)
12. washWashed twice more with ether
13. customto removed