반응 #2446058

반응 방정식

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]

반응 조건

후처리

1. 1
   온도The mixture is heated
2. 2
   온도After cooling
3. 3
   기타a yellow precipitate is collected
4. 4
   workup.ADDITION500 ml of a 1/1 ethanol/water mixture are added dropwise to the filtrate
5. 5
   기타The yellow paste obtained
6. 6
   기타is isolated
7. 7
   기타triturated with 200 ml of acetone
8. 8
   기타The solids obtained
9. 9
   세척are washed with 300 ml of water
10. 10
    기타dried
11. 11
    기타4.5 g of yellow powder are recovered

실험 절차

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.

출처