Reaktion #2509754

ord-499f028cfe444e09b3f4c60eccd4acd4

Reaktionsbedingungen

Temperatur
150°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to room temperature
  2. 2
    workup.DISTILLATIONdistilled water (100 ml)
  3. 3
    workup.ADDITIONwas added
  4. 4
    workup.STIRRINGstirred at that temperature for 1 hour
  5. 5
    FiltrationThe precipitated solid was taken out through filtration
  6. 6
    Sonstigedried
  7. 7
    Sonstigerecrystallized from hot ethanol

Vorschrift

2-Amino-N,3-dimethylbenzamide (4.10 g, 25.0 mmol), sodium hydrogensulfite (2.93 g, 27.5 mmol) and para-anisaldehyde (3.4 g, 25 mmol) were mixed in N,N′-dimethylacetamide (20 ml), stirred at 150° C. for 5 hours, then cooled to room temperature, and distilled water (100 ml) was added thereto and stirred at that temperature for 1 hour. The precipitated solid was taken out through filtration, dried, and recrystallized from hot ethanol to obtain the intended compound (3.42 g, 49%) as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07960394B2uspto-grants-2011_06