Reaktion #740346

ord-63806f4bb037423c8d3b5d3bf55b82a2

Reaktionsbedingungen

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

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is cooled
  2. 2
    Sonstigethe product isolated by the general procedure
  3. 3
    SonstigeThe excess hydrocarbons are removed by distillation at 190° C./0.04 mm
  4. 4
    SonstigeThe above-named product is obtained in a yield of 103.6 grams as a yellow liquid
  5. 5
    SonstigeThe liquid still contained inert hydrocarbon diluents which are removed by flash chromatography
  6. 6
    Sonstigeto give a pure product in a yield of 15 grams as a yellow liquid

Vorschrift

Using the general procedure of Example 1, 112 grams of 2-(2-hydroxy-5-methylphenyl)-2H-benzotriazole, 33 ml of methanesulfonic acid and 444 ml (2 moles) of a mixture of tetracosenes (prepared by the dimerization of n-dodecene) are heated at 160° C. for 96 hours. The reaction mixture is cooled and the product isolated by the general procedure described in Example 1. The excess hydrocarbons are removed by distillation at 190° C./0.04 mm. The above-named product is obtained in a yield of 103.6 grams as a yellow liquid. The liquid still contained inert hydrocarbon diluents which are removed by flash chromatography using silica gel and heptane/toluene 75/25 to give a pure product in a yield of 15 grams as a yellow liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04675352uspto-grants-1987_06