Reacción #51602
ord-c0e26b6ca5084e8b9c91033f3a1ae772
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1TemperaturaThe reaction mixture was heated
- 2Temperaturaat reflux for 3 hours
- 3Concentraciónconcentrated in vacuo
- 4TemperaturaThe concentrate was cooled to 5° C.
- 5FiltraciónThe solid was collected by filtration
- 6Lavadowashed with water
- 7Otrodried 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%).