Acetonitrile → 1,1'-(Disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide

Temperature

80 °C

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.

1. stirringThe mixture (white suspension) is kept stirring at 80° C. for 30 min
2. temperaturethe stirring is maintained at 80° C. for 90 min
3. temperatureAfter cooling
4. customthe solid obtained
5. filtrationis filtered off
6. washwashed with 100 ml of ACN
7. customdried
8. custom56.2 g of brown powder are recovered
9. temperatureat reflux
10. additionOnce the temperature has dropped to 40° C.
11. filtrationthe solid is filtered off
12. washwashed with 3 times 100 ml of iPrOH
13. customdried under vacuum

ORD record

ord-2a140e2d7035494484d0accf27d4cc9a

Source dataset

uspto-grants-2011_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08070830B2