Reaktion #2446058

Reaktionsgleichung

6-chloro-2-(2-{[2-(6-chloro-1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)ethyl]-disulphanyl}ethyl)-1H-benzo[de]isoquinoline-1,3(2H)-dione

N,N-dimethylpropane-1,3-diamine

→

2,2′-(Disulphanediyldiethane-2,1-diyl)bis[6-{[3-(dimethylamino)propyl]-amino}-1H-benzo[de]isoquinoline-1,3(2H)-dione]

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is heated
2. 2
   TemperaturAfter cooling
3. 3
   Sonstigea yellow precipitate is collected
4. 4
   workup.ADDITION500 ml of a 1/1 ethanol/water mixture are added dropwise to the filtrate
5. 5
   SonstigeThe yellow paste obtained
6. 6
   Sonstigeis isolated
7. 7
   Sonstigetriturated with 200 ml of acetone
8. 8
   SonstigeThe solids obtained
9. 9
   Waschenare washed with 300 ml of water
10. 10
    Sonstigedried
11. 11
    Sonstige4.5 g of yellow powder are recovered

Vorschrift

4 g of (6-chloro-2-(2-{[2-(6-chloro-1,3-dioxo-1H-benzo[de]isoquinolin-2(3H)-yl)ethyl]-disulphanyl}ethyl)-1H-benzo[de]isoquinoline-1,3(2H)-dione are suspended in 40 ml of N,N-dimethylpropane-1,3-diamine. The mixture is heated with stirring at 110° C. for 12 hours. After cooling, a yellow precipitate is collected, and 500 ml of a 1/1 ethanol/water mixture are added dropwise to the filtrate. The yellow paste obtained is isolated and triturated with 200 ml of acetone. The solids obtained are washed with 300 ml of water and dried. 4.5 g of yellow powder are recovered. The analyses show that the product is in accordance with the expected product.

Quelle