반응 #742267

반응 방정식

acetonitrile

1-bromo-2-[(2-bromoethyl)-disulphanyl]ethane

N-methylpyrrolidone

2-picoline

→

light beige product

1,1′-(disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide

반응 조건

후처리

1. 1
   workup.STIRRINGThe mixture (white suspension) is kept stirring at 80° C. for 30 min
2. 2
   온도the stirring is maintained at 80° C. for 90 min
3. 3
   온도After cooling
4. 4
   기타the solid obtained
5. 5
   여과is filtered off
6. 6
   세척washed with 100 ml of ACN
7. 7
   기타dried
8. 8
   기타56.2 g of brown powder are recovered
9. 9
   온도at reflux
10. 10
    workup.ADDITIONOnce the temperature has dropped to 40° C.
11. 11
    여과the solid is filtered off
12. 12
    세척washed with 3 times 100 ml of iPrOH
13. 13
    기타dried under vacuum

실험 절차

A mixture of 56 g of 1-bromo-2-[(2-bromoethyl)-disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) is poured dropwise onto 35 g of 2-picoline with stirring, at 80° C. The mixture (white suspension) is kept stirring at 80° C. for 30 min, 100 ml of acetonitrile (ACN) are added, and the stirring is maintained at 80° C. for 90 min. After cooling, the solid obtained is filtered off, washed with 100 ml of ACN and then dried. 56.2 g of brown powder are recovered. 45 g of this powder are suspended in 300 ml of isopropanol (iPrOH), at reflux. Once the temperature has dropped to 40° C., the solid is filtered off, washed with 3 times 100 ml of iPrOH and dried under vacuum. 40.56 g of a light beige product are obtained. The analyses are in conformity with the expected structure.

출처