Reaktion #416070

ord-c98a98829b754cf5b58e24ee459cdcd4

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    TemperaturThe reaction mixture was cooled
  3. 3
    Extraktionextracted with ether
  4. 4
    WaschenThe extract was washed with 2N-NaOH aqueous solution
  5. 5
    TrocknenThe liquid was dried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONthe solvent was distilled off
  7. 7
    SonstigeRecrystallization of the residue

Vorschrift

To a mixture of 14.2 parts of 1-(sec.-butyl-3-azetidinol and 14.4 parts of α-naphthol 0.2 part of sodium hydroxide was added and the mixture was heated under nitrogen gas at 160° C. for 22 hours. The reaction mixture was cooled and then extracted with ether. The extract was washed with 2N-NaOH aqueous solution and then with water. The liquid was dried over anhydrous sodium sulfate and the solvent was distilled off. Recrystallization of the residue gave 15.5 parts of 1-(α-naphthoxy)-3-(sec.-butylamino)-2-propanol melting at 57°-59° C. The yield was 57%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04018824uspto-grants-1977_04