Reaction #41510

ord-4d438631632e491eab1ba9bb43893932

Conditions

Temperature
50°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperaturewhile heating to 85° C.
  2. 2
    Otherstirring at 85° C.
  3. 3
    TemperatureThe reaction mixture is cooled

Procedure

1 020 g (10 mol) of dimethylaminopropylamine and 267.5 g (2.5 mol) of benzylamine are mixed in 1 519.1 g of water. The solution/suspension is heated to 50° C. Thereafter, 931 ml of epichlorohydrin (1 098.4 g/l 1.875 mol) are added dropwise at a rate of 16 ml/min while heating to 85° C., and stirring is effected for two hours at 85° C. The stirring at 85° C. is continued until free alkylating agent is no longer detectable (Preuβmann test). The reaction mixture is cooled, diluted with 2 l of water and brought to a pH of 7.0 with 85% strength formic acid. Further water is added until the solids content is 21%.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728072B2uspto-grants-2010_06