Reacción #51602

ord-c0e26b6ca5084e8b9c91033f3a1ae772

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe reaction mixture was heated
  2. 2
    Temperaturaat reflux for 3 hours
  3. 3
    Concentraciónconcentrated in vacuo
  4. 4
    TemperaturaThe concentrate was cooled to 5° C.
  5. 5
    FiltraciónThe solid was collected by filtration
  6. 6
    Lavadowashed with water
  7. 7
    Otrodried in vacuo at 35-40° C.

Procedimiento

A mixture of 5B (2.38 g) and methanol (20 ml) was added to a stirred solution of sodium hydroxide (1.68 g) in water (20 ml). The reaction mixture was heated at reflux for 3 hours. The reaction mixture was cooled to room temperature and concentrated in vacuo. The concentrate was cooled to 5° C. and acidified with concentrated HCl (3.5 ml). The resulting suspension was stirred at 5° C. for 30 minutes. The solid was collected by filtration, washed with water, then dried in vacuo at 35-40° C. to give the free acid (1.45 g, 65%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06852673B2uspto-grants-2005_02