Reacción #2267076

Ecuación de reacción

14

6-Acetylamino-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

→

desired product 15

Rendimiento 100.0%

6-Amino-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

Rendimiento 100.0%

Disolventes

H2SO4

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaAfter refluxing for 15 hours
2. 2
   Otrothe methanol was removed under reduced pressure
3. 3
   Extracciónfollowed by extraction with ethyl acetate three times
4. 4
   SecadoThe combined organic phase was dried over Na2SO4
5. 5
   OtroRemoval of the solvent

Procedimiento

Solution of 14 (0.114 g, 0.32 mmol) in 5 ml of 4N H2SO4 and 5 ml of methanol was heated to reflux. After refluxing for 15 hours, the methanol was removed under reduced pressure. The remaining aqueous solution was neutralized with NaHCO3 to pH 9, followed by extraction with ethyl acetate three times. The combined organic phase was dried over Na2SO4. Removal of the solvent afforded the desired product 15 (100 mg, 100%) which was used directly for next step.

Fuente