Reaktion #684729

ord-114a87da323340c78ecb48e6ebd53b91

Reaktionsgleichung

CC1(C)CC(O)CC(C)(C)N1
2,2,6,6-tetramethylpiperidin-4-ol
CCCCCCCCCCCCBr
n-dodecyl bromide
CCCCCCCCCCCCN1C(C)(C)CC(O)CC1(C)C
1-n-dodecyl-2,2,6,6-tetramethylpiperidin-4-ol

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated under reflux conditions for 72 hours
  2. 2
    SonstigeThe cooled reaction mixture
  3. 3
    Filtrationwas filtered
  4. 4
    Sonstigeto remove 2,2,6,6-tetramethylpiperidin-4-ol hydrobromide
  5. 5
    Sonstigeformed during the reaction
  6. 6
    Sonstigethe ethyl alcohol solvent was removed by distillation under reduced pressure
  7. 7
    workup.ADDITIONThe residue was treated with petroleum under (b.p. 40°-60°C)
  8. 8
    Filtrationfiltered
  9. 9
    Sonstigeto remove the unreacted 2,2,6,6-tetramethylpiperidin-4-ol
  10. 10
    Sonstigethe petroleum ether solvent was removed by distillation under reduced pressure
  11. 11
    workup.DISTILLATIONFractional distillation of the residue

Vorschrift

A mixture of 15.7 parts of 2,2,6,6-tetramethylpiperidin-4-ol and 12.5 parts of n-dodecyl bromide in 50 parts of ethyl alcohol was heated under reflux conditions for 72 hours. The cooled reaction mixture was filtered to remove 2,2,6,6-tetramethylpiperidin-4-ol hydrobromide formed during the reaction and the ethyl alcohol solvent was removed by distillation under reduced pressure. The residue was treated with petroleum under (b.p. 40°-60°C) and filtered to remove the unreacted 2,2,6,6-tetramethylpiperidin-4-ol and the petroleum ether solvent was removed by distillation under reduced pressure. Fractional distillation of the residue gave 1-n-dodecyl-2,2,6,6-tetramethylpiperidin-4-ol having a melting point of 41°-2°C and the following elemental analysis by weight:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04014887uspto-grants-1977_03