Reaktion #1972828

ord-5848a999af7d432982abc2d99af019a7

Reaktionsbedingungen

Temperatur
125°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter 8 hours it is cooled down
  2. 2
    workup.DISTILLATIONthe excess 1-methylpiperazine is distilled off
  3. 3
    Extraktionthe mixture is extracted with dilute hydrochloric acid
  4. 4
    Extraktionis extracted with toluene
  5. 5
    TrocknenThe toluene solution is dried with K2CO3
  6. 6
    Einengenconcentrated
  7. 7
    SonstigeThe residue, 29.4 g of a cognac-coloured oil, is then further reacted

Vorschrift

29.43 g (0.15 mol) of 2-(4-fluorophenyl)-3,3-dimethyl-2-methoxyoxirane and 60.1 g (0.60 mol) of 1-methylpiperazine are brought together, and the mixture is heated to about 125° C. After 8 hours it is cooled down and the excess 1-methylpiperazine is distilled off. The residue is taken up in toluene, and the mixture is extracted with dilute hydrochloric acid. The hydrochloric acid solution is rendered alkaline and is extracted with toluene. The toluene solution is dried with K2CO3 and concentrated. The residue, 29.4 g of a cognac-coloured oil, is then further reacted.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05145885uspto-grants-1992_09