Reacción #59053

ord-db7085d42a274783a30f20534fc66b50

Disolventes

Condiciones de reacción

Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaheated
  2. 2
    Temperaturaunder reflux at 100° C. for 7.5 hrs
  3. 3
    Temperaturaheated
  4. 4
    Temperaturaunder reflux for 16 hrs
  5. 5
    TemperaturaAfter being cooled to room temperature
  6. 6
    Filtraciónthe precipitate was collected by filtration

Procedimiento

A 2 mol/L aqueous solution of sodium hydroxide (0.43 mL) was added to a solution of ethyl 4′-(2-[(1S,2R)-2-hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy)biphenyl-4-carboxylate (0.15 g), ethanol (20 mL) and tetrahydrofuran (5 mL). The mixture was stirred at 60° C. for 16 hrs, and heated under reflux at 100° C. for 7.5 hrs. A 2 mol/L aqueous solution of sodium hydroxide (0.17 mL) was added, and heated under reflux for 16 hrs. After being cooled to room temperature, 2 mol/L hydrochloric acid (0.60 mL) was added, and the precipitate was collected by filtration to afford the title compound as a pale yellow amorphous (0.13 g). The structure and physical data were shown in table 3.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07423185B2uspto-grants-2008_09