Reaction #2446057

Reaction equation

N-methylpyrrolidone

6-chloro-1H,3H-benzo[de]isochromene-1,3-dione

cystamine hydrochloride

NMP

diisopropylethylamine

→

2,2′-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)

Conditions

Workup

1. 1
   Temperaturethe mixture is heated
2. 2
   workup.STIRRINGwith stirring at 120° C. for 3 hours
3. 3
   TemperatureAfter cooling
4. 4
   Otherthe precipitated product is recovered
5. 5
   workup.ADDITIONthe filtered solution is extended by addition of 200 ml of water
6. 6
   Othera second precipitate is recovered
7. 7
   WashThe precipitates are washed with water
8. 8
   Otherdried
9. 9
   Other11.46 g of white powder are recovered

Procedure

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1,3-dione and 4.46 g of hydrochlorided cystamine hydrochloride are suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine are added and the mixture is heated with stirring at 120° C. After two hours, 50 ml of NMP are added and the mixture is kept with stirring at 120° C. for 3 hours. After cooling, the precipitated product is recovered and the filtered solution is extended by addition of 200 ml of water, and a second precipitate is recovered. The precipitates are washed with water and dried. 11.46 g of white powder are recovered. The analyses show that the product is in accordance with the expected product.

Source