Reaktion #6260

ord-eada9dfe6c2247098ac3fc6740df3411

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Filtrationthe insoluble material was filtered off
  3. 3
    workup.DISTILLATIONThe volatile components were distilled off
  4. 4
    workup.ADDITIONchloroform was added to the residue
  5. 5
    WaschenThe mixture was washed with saturated saline
  6. 6
    Trocknendried over potassium carbonate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off

Vorschrift

To a suspension of 12.50 g (40 mmol) of 4-(4-phthalimidobutylthio)pyridine in 200 ml of ethanol, 5.82 ml (120 mmol) of hydrazine monohydrate was added, and the mixture was stirred at room temperature for 4 hours. Then, 200 ml of ethyl acetate was-added, and the insoluble material was filtered off. The volatile components were distilled off and chloroform was added to the residue. The mixture was washed with saturated saline and dried over potassium carbonate. The solvent was distilled off and 7.30 g of the desired compound were obtained (quantitative yield, yellow oil).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05246948uspto-grants-1993_09