Reacción #61058

ord-2e3edcb0c82b451dbae29a3aae31849e

Reactivos

Ninguno

Condiciones de reacción

Temperatura
2.5°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroA 1 L 3-necked round bottom flask was equipped with a mechanical stirrer
  2. 2
    TemperaturaThe reaction mixture was heated
  3. 3
    Temperaturato reflux for 3 hours
  4. 4
    FiltraciónThe crystalline solid was collected by vacuum filtration
  5. 5
    Lavadowashed with ether
  6. 6
    OtroThe solid product was dried in vacua at ambient temperature to a constant weight

Procedimiento

A 1 L 3-necked round bottom flask was equipped with a mechanical stirrer, thermometer, and condenser and charged with 3-aminophthalic acid (108 g, 596 mmol) and acetic anhydride (550 mL). The reaction mixture was heated to reflux for 3 hours and cooled to ambient temperature and further to 0-5° C. for another 1 hour. The crystalline solid was collected by vacuum filtration and washed with ether. The solid product was dried in vacua at ambient temperature to a constant weight, giving 75 g (61% yield) of 3-acetamidopthalic anhydride as a white product. 1H-NMR (CDCl3) δ: 2.21 (s, 3H), 7.76 (d, 1H), 7.94 (t, 1H), 8.42 (d, 1H), 9.84 (s, 1H).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07427638B2uspto-grants-2008_09