Reaktion #1853335

Reaktionsgleichung

1-chloroisoquinoline

sodium hydride

1H-pyrrolo[2,3-b]pyridine

→

1-(isoquinolin-1-yl)-1H-pyrrolo[2,3-b]pyridine

Ausbeute 52.5%

Lösungsmittel

dimethylformamide

dimethylformamide

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe reaction mixture was heated at a temperature in the region of 100° C. for 15 h
2. 2
   EinengenAfter concentrating to dryness under reduced pressure (2.7 kPa)
3. 3
   SonstigeThe white crystals that formed
4. 4
   Filtrationwere filtered off
5. 5
   Sonstigedried under reduced pressure (2.7 kPa) at a temperature in the region of 20° C

Vorschrift

0.894 g of 60% sodium hydride (37.25 mmol) was added with stirring to 20 cm3 of dimethylformamide under an argon atmosphere at a temperature in the region of 20° C. and then a solution of 4 g (33.86 mmol) of 1H-pyrrolo[2,3-b]pyridine in 20 cm3 of dimethylformamide was gradually added. After stirring at a temperature in the region of 20° C. for 30 minutes, a solution of 5.816 g (35.55 mmol) of 1-chloroisoquinoline in 20 cm3 of dimethylformamide was added and then the reaction mixture was heated at a temperature in the region of 100° C. for 15 h. After concentrating to dryness under reduced pressure (2.7 kPa), the residue was taken up in 2 times 50 cm3 of water. The residual oil was taken up in 30 cm3 of diethyl ether. The white crystals that formed were filtered off and then dried under reduced pressure (2.7 kPa) at a temperature in the region of 20° C. 4.36 g of 1-(isoquinolin-1-yl)-1H-pyrrolo[2,3-b]pyridine were thus obtained in the form of an off-white solid melting at 87° C.

Quelle