Reaktion #703703

Reaktionsgleichung

carbon dioxide

2,2'-diazidobiphenyl

ethyl alcohol

→

benzo[C]cinnoline

Ausbeute 52.0%

Lösungsmittel

glycerol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe solution thus obtained
2. 2
   SonstigeThe cell was irradiated with light in the same manner
3. 3
   SonstigeAfter the irradiation
4. 4
   Extraktionthe reaction product was extracted with 2l of diethyl ether
5. 5
   SonstigeDiethyl ether was removed off by distillation

Vorschrift

160 mg of 2,2'-diazidobiphenyl was dissolved in a small amount of diethyl ehter and then the solution thus obtained was dissolved in 500 ml of glycerol and the resultant solution was poured into a quarty cylindrical cell. The cell was dipped into a mixed coolant of ethyl alcohol and solid carbon dioxide to convert the solution to low-temperature rigid solution. The cell was irradiated with light in the same manner set forth in Example 1. After the irradiation, the cell was taken out of the coolant. After fluidized, the reaction product was extracted with 2l of diethyl ether. Diethyl ether was removed off by distillation. 62 mg of pure benzo[C]cinnoline was obtained by recrystallization of the residue using a mixed solvent of hexane and diethyl ether. Yield was about 52%.

Quelle