Réaction #60570

ord-b4cf512b24414ddb88ba1145d2c5719a

Conditions de réaction

Température
80°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    ConcentrationAfter concentration
  2. 2
    Autreby evaporation under vacuum, it
  3. 3
    Extractionextracted three times with 25 ml each of methylene chloride
  4. 4
    AutreThe collected organic phase is dried
  5. 5
    Filtrationfiltered
  6. 6
    Concentrationconcentrated by evaporation, and 145 mg (32% of theory) of [2-(4-acetylamino-2-methoxy-benzoylamino)-ethyl]-diethyl-methyl-ammonium iodide with a melting point >300° C.
  7. 7
    Autreis obtained

Mode opératoire

307 mg (1, mmol) of 4-acetylamino-N-(2-diethylamino-ethyl)-2-methoxy-benzamide is mixed in 8 ml of dimethylformamide with 358 mg (1.1 mmol) of cesium carbonate and 312 mg (2.2 mmol) of iodomethane, and it is heated under argon in a pressure vessel for 2.5 hours to a bath temperature of 80° C. After concentration by evaporation under vacuum, it is taken up in 25 ml of saturated sodium bicarbonate solution and extracted three times with 25 ml each of methylene chloride. The collected organic phase is dried, filtered and concentrated by evaporation, and 145 mg (32% of theory) of [2-(4-acetylamino-2-methoxy-benzoylamino)-ethyl]-diethyl-methyl-ammonium iodide with a melting point >300° C. is obtained.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07427390B2uspto-grants-2008_09