Reaction #2446056

ord-b642f1eab236411891d81753ec7ef95f

Reaction equation

CC#N
acetonitrile
BrCCSSCCBr
1-bromo-2-[(2-bromoethyl)disulphanyl]ethane
CN1CCCC1=O
N-methylpyrrolidone
Cc1ccccn1
2-picoline
Cc1cccc[n+]1CCSSCC[n+]1ccccc1C.[Br-].[Br-]
1,1′-(Disulphanediyldiethane-2,1-diyl)bis(2-methylpyridinium)dibromide

Conditions

Temperature
80°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.STIRRINGwith stirring at 80° C. for 30 minutes
  2. 2
    workup.STIRRINGstirring
  3. 3
    Temperatureis maintained at 80° C. for 90 minutes
  4. 4
    TemperatureAfter cooling
  5. 5
    Otherthe solid obtained
  6. 6
    Filtrationis filtered off
  7. 7
    Washwashed with 100 ml of acetonitrile
  8. 8
    Otherdried

Procedure

A mixture of 56 g of 1-bromo-2-[(2-bromoethyl)disulphanyl]ethane and 15 ml of N-methylpyrrolidone (NMP) is introduced dropwise into 35 g of 2-picoline with stirring at 80° C. The mixture (white suspension) is kept with stirring at 80° C. for 30 minutes, 100 ml of acetonitrile are added, and stirring is maintained at 80° C. for 90 minutes. After cooling, the solid obtained is filtered off, washed with 100 ml of acetonitrile and then dried.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08685114B2uspto-grants-2014_04