Reaktion #437844

ord-85a751e6f4dd4ce391463003e52e8d36

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with saturated sodium hydrogen carbonate solution
  2. 2
    TrocknenThe combined organic phases are dried over magnesium sulphate
  3. 3
    Sonstigeevaporated down
  4. 4
    SonstigeThe solid, yellowish crude product is triturated with tert.-butylmethylether, suction
  5. 5
    Filtrationfiltered
  6. 6
    Waschenwashed with tert.-butylmethylether
  7. 7
    Sonstigedried

Vorschrift

A solution of 300 mg of 1-chloromethyl-3-methyl-isoquinoline in 3 ml of methylene chloride is combined with 390 mg of 3-chloroperoxybenzoic acid and stirred overnight at ambient temperature. The reaction mixture is diluted with some methylene chloride and extracted with saturated sodium hydrogen carbonate solution. The combined organic phases are dried over magnesium sulphate and evaporated down. The solid, yellowish crude product is triturated with tert.-butylmethylether, suction filtered, washed with tert.-butylmethylether and dried.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07183280B2uspto-grants-2007_02