Reaktion #798808

ord-69a0d9ea05ba4acfaaee5b555d7a9fe9

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe reaction
  2. 2
    Waschenwashed with water and brine
  3. 3
    TrocknenThe ethyl acetate portion was dried over sodium sulfate and solvent
  4. 4
    Sonstigewas evaporated under reduced pressure
  5. 5
    Sonstigethe product was purified by prep HPLC

Vorschrift

To a mixture of 2-(benzylamino)-4,5-dimethylthiophene-3-carbonitrile (302 mg, 2.0 mmol), potassium carbonate (276 mg, 2.0 mmol), and a catalytic amount of potassium iodide in acetonitrile (1 mL) in a 20 mL microwave vial was added ethyl iodide (310 mg, 2.0 mmol). The reaction vial was placed in a microwave reactor for 15 minutes at 165° C. The reaction mixture was dissolved in ethyl acetate and washed with water and brine. The ethyl acetate portion was dried over sodium sulfate and solvent was evaporated under reduced pressure, and the product was purified by prep HPLC using acetonitrile/water as solvent. MS 181 (MH+).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09181276B2uspto-grants-2015_11