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)disulfanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) was poured dropwise over 35 g of 2-picoline with stirring at 80° C. The mixture (white suspension) continued to be stirred for 30 min at 80° C., then 100 ml of acetonitrile were added and the stirring was continued at 80° C. for 90 min. After cooling, the solid obtained was filtered, washed with 100 ml of acetonitrile, then dried. 56.2 g of brown powder were recovered. 45 g of this powder were suspended in 300 ml of isopropanol, under reflux. Once the temperature dropped to 40° C., the solid was filtered, washed with three times 100 ml of isopropanol and dried under vacuum. Thus, 40.56 g of a light beige product was obtained. Analyses were in accordance with the expected structure.

1. stirringto be stirred for 30 min at 80° C.
2. temperatureAfter cooling
3. customthe solid obtained
4. filtrationwas filtered
5. washwashed with 100 ml of acetonitrile
6. customdried
7. custom56.2 g of brown powder were recovered
8. temperatureunder reflux
9. additionOnce the temperature dropped to 40° C.
10. filtrationthe solid was filtered
11. washwashed with three times 100 ml of isopropanol
12. customdried under vacuum

ORD record

ord-be580d6107a34e46ace26a1080ca1113

Source dataset

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08097044B2