반응 #553077

반응 방정식

cysteamine

succinic anhydride

N-(2-mercapto ethyl) succinamic acid

cystamine

→

N-(2-mercapto ethyl) succinimide

용매

water

반응 조건

후처리

1. 1
   기타the cyclization reaction
2. 2
   기타At the end of the reaction
3. 3
   온도the mixture is cooled
4. 4
   기타7 g of crude product are obtained
5. 5
   workup.ADDITIONare added
6. 6
   workup.STIRRINGAfter stirring for one hour
7. 7
   기타having reacted
8. 8
   기타is removed by filtration
9. 9
   workup.ADDITIONthere are added to the stirred filtrate, 10 g of sulfonic resin and 3 g of zinc powder
10. 10
    여과After 3 hours the mixture is filtered
11. 11
    농축the filtrate is concentrated under reduced pressure
12. 12
    기타After drying

실험 절차

About one-half hour is necessary for the complete transformation of the succinic anhydride (V.P.C.). At this stage, to facilitate the cyclization reaction, the reaction mixture is placed under reduced pressure and the evolution of the reaction mixture is followed by acidimetric dosage of the nontransformed N-(2-mercapto ethyl) succinamic acid. At the end of the reaction, the mixture is cooled and 7 g of crude product are obtained and dissolved in 50 cm3 of water to which are added, with stirring, 10 g of sulfonic acid resin. After stirring for one hour, the resin, having fixed the traces of cysteamine or cystamine not having reacted, is removed by filtration. To reduce the disulfide optionally present, there are added to the stirred filtrate, 10 g of sulfonic resin and 3 g of zinc powder. After 3 hours the mixture is filtered and the filtrate is concentrated under reduced pressure. After drying, 5 g of N-(2-mercapto ethyl) succinimide are obtained in the form of a white powder whose melting point is 45° C.

출처