Reaktion #1941578

ord-0d1f16dc4f694207bc0b2d7cf83583de

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe reaction mixture was cooled to ambient temperature
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Waschenwashed with water (10 mL)
  4. 4
    Trocknendried over anhydrous Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated under reduced pressure

Vorschrift

To a solution of 1-cyclohexyl-6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine (0.020 g, 0.051 mmol) in 1,4-dioxane (3 mL) was added aqueous NaOH (2 N, 0.380 mL, 0.760 mmol). The reaction mixture was heated to about 90° C. After about 5 h, the reaction mixture was cooled to ambient temperature and diluted with EtOAc (10 mL) and saturated aqueous NH4Cl (10 mL). The organic layer was separated and washed with water (10 mL) followed by brine (10 mL), dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure to provide 1-cyclohexyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazine as a tan solid (0.011 g, 90%): LC/MS (Table 2, Method a) Rt=1.92 min; MS m/z: 241 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08962629B2uspto-grants-2015_02