Реакция #507595

Уравнение реакции

N-methylpyrrolidone

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

cystamine hydrochloride

NMP

diisopropylethylamine

→

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

Условия реакции

Обработка

1. 1
   Температураthe mixture was heated
2. 2
   workup.STIRRINGto be stirred at 120° C. for 3 h
3. 3
   ТемператураAfter cooling
4. 4
   Другоеthe precipitated product was recovered
5. 5
   workup.ADDITIONthe filtered solution was extended by addition of 200 ml of water
6. 6
   Другоеa second precipitate was recovered
7. 7
   ПромывкаThe precipitates were washed in water
8. 8
   Другоеdried
9. 9
   Другое11.46 g of white powder were recovered

Методика

9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1,3-dione and 4.46 g of cystamine hydrochloride were suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine were added and the mixture was heated, with stirring, at 120° C. After 2 hours, 50 ml of NMP were added and the mixture continued to be stirred at 120° C. for 3 h. After cooling, the precipitated product was recovered, the filtered solution was extended by addition of 200 ml of water and a second precipitate was recovered. The precipitates were washed in water and dried. 11.46 g of white powder were recovered. The analyses showed that the product conformed to the expected structure.

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