Reaktion #220373

Reaktionsgleichung

3-(2-chloro-4-bromophenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one

NMP

CuCN

→

expected compound

3-(2,4-Dicyanophenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture is heated
2. 2
   Temperaturat reflux for 5 hours
3. 3
   workup.ADDITIONThe reaction medium is poured onto CH2Cl2
4. 4
   Waschenwashing
5. 5
   SonstigePurification
6. 6
   Wascheneluted with an AcOEt/petroleum ether (v/v; 75/25) mixture
7. 7
   SonstigeThe fractions recovered
8. 8
   Waschenare washed with a 1N HCl solution
9. 9
   Sonstigeto remove an NMP residue

Vorschrift

0.6 g of 3-(2-chloro-4-bromophenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one is dissolved in 15 ml of NMP. 0.27 g of CuCN is added and then the mixture is heated at reflux for 5 hours. The reaction medium is poured onto CH2Cl2 and washing is carried out with a saturated NaCl solution. Purification is carried out by chromatography on a silica column eluted with an AcOEt/petroleum ether (v/v; 75/25) mixture and then pure AcOEt. The fractions recovered are washed with a 1N HCl solution to remove an NMP residue. 50 mg of the expected compound are obtained in the form of a powder.

Quelle