Reaktion #433168

ord-6ec7564c092242d599acd3e691bce00e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for 4 hours
  2. 2
    Temperaturat reflux
  3. 3
    workup.STIRRINGare vigorously stirred until the precipitated salt
  4. 4
    SonstigeThe aqueous phase is separated off
  5. 5
    Waschenthe xylene solution is washed three times
  6. 6
    Sonstigeeach with 100 ml of water, and evaporated in vacuo
  7. 7
    SonstigeThe oily residue is dried at 100°

Vorschrift

20.5 g of 2,4-dichloro-6-(2,2,6,6-tetramethyl-4-benzoyloxypiperidin-1-yl)-1,3,5-triazine (prepared according to Example 2) are stirred in 200 ml of xylene with 8.0 g of n-butylamine at reflux for 4 hours. 4.4 g of pulverized sodium hydroxide are added to the reaction mixture and it is stirred for a further 15 hours at reflux. The contents of the flask are cooled to room temperature and, after addition of 100 ml of water, are vigorously stirred until the precipitated salt has completely gone into solution. The aqueous phase is separated off, and the xylene solution is washed three times, each with 100 ml of water, and evaporated in vacuo. The oily residue is dried at 100° and 13 Pa. 2,4-Bis-butylamino-6-(2,2,6,6-tetramethyl-4-benzoylpiperidin-1-yl)-1,3,5-triazine is obtained as a yellowish viscous material.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05059689uspto-grants-1991_10