Reaktion #75589

ord-635d4e8135284b9c843e3b279e4f9469

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Waschenwas washed with water for 3 times
  3. 3
    Trocknenwith brine, dried over anhydrous magnesium sulfate
  4. 4
    Filtrationfiltered
  5. 5
    SonstigeThe filtrate was evaporated

Vorschrift

4.25 g of tert-butyl 1-oxa-6-azaspiro[2.5]octane-6-carboxylate was dissolved in 30 ml dimethylformamide, 5.38 g of sodium imidazole was added thereto, and the mixture was stirred at 60° C. for 3 hr and 40 min. After cooling, ethyl acetate was added to the reaction solution, and it was washed with water for 3 times and then with brine, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated and subjected to silica gel column chromatography to give 4.93 g of tert-butyl 4-hydroxy-4-(1H-1-imidazolylmethyl)-1-piperidinecarboxylate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06699870B2uspto-grants-2004_03