Реакция #2446058

Уравнение реакции

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]

Условия реакции

Обработка

1. 1
   ТемператураThe mixture is heated
2. 2
   ТемператураAfter cooling
3. 3
   Другоеa yellow precipitate is collected
4. 4
   workup.ADDITION500 ml of a 1/1 ethanol/water mixture are added dropwise to the filtrate
5. 5
   ДругоеThe yellow paste obtained
6. 6
   Другоеis isolated
7. 7
   Другоеtriturated with 200 ml of acetone
8. 8
   ДругоеThe solids obtained
9. 9
   Промывкаare washed with 300 ml of water
10. 10
    Другоеdried
11. 11
    Другое4.5 g of yellow powder are recovered

Методика

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.

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