Reaktion #56537

ord-a743ed6fe47347c5aeb58ad11b43992b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONis added dropwise at 10° C.
  2. 2
    Temperaturheated on a steam bath for another 30 minutes
  3. 3
    SonstigeThe precipitate formed
  4. 4
    Filtrationis filtered
  5. 5
    Waschenthe filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution
  6. 6
    Trocknendried over magnesium sulfate
  7. 7
    SonstigeThe solvent is evaporated
  8. 8
    Sonstigeto give 41.3 g

Vorschrift

To a mixture of 2-cyano-2-(2,4-dichlorophenyl)decan-1-ol (40 g., 0.12 mole) and methane sulfonyl chloride (15.3 g., 0.13 mole) in 2 liters of benzene is added dropwise at 10° C., 14.8 g., (0.14 mole) of triethylamine. The reaction mixture is stirred at room temperature for 30 minutes and then heated on a steam bath for another 30 minutes. The precipitate formed is filtered and the filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution and dried over magnesium sulfate. The solvent is evaporated to give 41.3 g. of product, which is identified by nmr.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225723uspto-grants-1980_09