反应详情

温度

60 °C

6-Nitro-2,2-dimethyl-4H-benzo[1,3]dioxin-4-one (5 g, 22.42 mmol) was taken up in EtOH (35 ml) and 10% Pd on C (wet basis) (2.37 g) was added. The mixture was hydrogenated at 50 psi for 1 hr. The mixture was filtered through celite and the volatiles were removed in vacuo. IPA (50 ml) was added and the mixture was heated at 60° C. for 5 mins then allowed to cool to RT. The resulting solid was filtered off, washed with MTBE and dried in vacuo to give 2.93 g of 6-amino-2,2-dimethyl-4H-benzo[1,3]dioxin-4-one (68%) as a yellow solid.

1. filtrationThe mixture was filtered through celite
2. customthe volatiles were removed in vacuo
3. additionIPA (50 ml) was added
4. temperatureto cool to RT
5. filtrationThe resulting solid was filtered off
6. washwashed with MTBE
7. customdried in vacuo