Reaktion #2046064

ord-52f897bef7384d609ac7015eafa40d33

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was evaporated in vacuo and water
  2. 2
    workup.ADDITIONwas added to the crude residue
  3. 3
    SonstigeThe dark solid precipitated
  4. 4
    Filtrationwas filtered
  5. 5
    Sonstigedried
  6. 6
    Sonstigeyielding a crude product
  7. 7
    Sonstigepurified by crystallization in ethyl acetate

Vorschrift

A mixture of 2-chloro-N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)acetamide (0.22 g, 0.74 mmol), morpholine (71 mg, 0.81 mmol), potassium carbonate (0.22 g, 1.62 mmol) and sodium iodide (0.11 g, 0.74 mmol) in dry dimethylformamide (5 ml) was stirred and warmed at 100° C., overnight, in a dry nitrogen atmosphere. The solvent was evaporated in vacuo and water was added to the crude residue. The dark solid precipitated was filtered and dried yielding a crude product purified by crystallization in ethyl acetate, and 0.23 g of N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide was obtained as a beige colour solid with m.p.=125-127° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08410159B2uspto-grants-2013_04