Reacción #443137
ord-6b3c2d17ec114522a26bbf4377b5a763
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1TemperaturaAfter cooling the solution
- 2Temperaturawhile maintaining the internal temperature below 5° C
- 3OtroThe resultant reaction mixture
- 4workup.ADDITIONwas poured into ice-
- 5Extracciónextracted with chloroform
- 6LavadoThe extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order
- 7Secadodried over anhydrous sodium sulfate
- 8OtroThe solvent was evaporated
- 9Otroresidue was recrystallized in methanol
Procedimiento
14 gm of the compound prepared in (7) above was dissolved into 100 ml of concentrated sulfuric acid. After cooling the solution, a solution of 9.05 gm of potassium nitrate in 80 ml of concentrated sulfuric acid was added dropwise while maintaining the internal temperature below 5° C. The stirring was continued for a further 30 minutes. The resultant reaction mixture was poured into ice-cooled water and extracted with chloroform. The extract was washed with saturated aqueous solution of sodium bicarbonate, water, and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated and residue was recrystallized in methanol to obtain 9.15 gm of the title compound.