反应 #2446058

反应方程式

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]

反应条件

后处理

1. 1
   温度The mixture is heated
2. 2
   温度After cooling
3. 3
   其他a yellow precipitate is collected
4. 4
   workup.ADDITION500 ml of a 1/1 ethanol/water mixture are added dropwise to the filtrate
5. 5
   其他The yellow paste obtained
6. 6
   其他is isolated
7. 7
   其他triturated with 200 ml of acetone
8. 8
   其他The solids obtained
9. 9
   洗涤are washed with 300 ml of water
10. 10
    其他dried
11. 11
    其他4.5 g of yellow powder are recovered

实验过程

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.

来源