反応 #2446058

反応方程式

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]

反応条件

後処理

1. 1
   温度The mixture is heated
2. 2
   温度After cooling
3. 3
   その他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
   その他The yellow paste obtained
6. 6
   その他is isolated
7. 7
   その他triturated with 200 ml of acetone
8. 8
   その他The solids obtained
9. 9
   洗浄are washed with 300 ml of water
10. 10
    その他dried
11. 11
    その他4.5 g of yellow powder are recovered

実験手順

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.

出典