Reaktion #1616729

ord-50c95e5fcbbb40319520a0bd04e6e757

Lösungsmittel

Reaktionsbedingungen

Temperatur
170°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with DCM
  2. 2
    SonstigeThe organic layer was separated
  3. 3
    Trocknendried (Na2SO4)
  4. 4
    Filtrationfiltered
  5. 5
    Sonstigethe solvents evaporated in vacuo

Vorschrift

Lithium hydroxide (0.66 g, 27.7 mmol) was added to a stirred solution of 6,7-dihydro-2-(phenoxymethyl)-oxazolo[5,4-c]pyridine-5(4H)-carboxylic acid ethyl ester (1.77 g, 5.55 mmol) in a mixture of H2O (5 mL) and 1,4-dioxane (15 mL) under N2. The mixture was stirred at 170° C. for 40 minutes under microwave irradiation, diluted with H2O and extracted with DCM. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield 4,5,6,7-tetrahydro-2-(phenoxymethyl)-oxazolo[5,4-c]pyridine (0.58 g, 45% yield) as a purple oil that was used in the next step without further purification. C13H14N2O2 LCMS: Rt 1.07, m/z 231 [M+H]+ (using method, LC-MS Method 6).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09090632B2uspto-grants-2015_07