反应详情

3,3-Diethyl-1-methyl-5-nitro-1,3-dihydro-indol-2-one (9.3 g) is dissolved in acetic acid (100 ml) and subjected to a catalytic hydrogenation with Raney-nickel (1 g) at 3 bar. After completion of the hydrogenation the mixture is filtered and evaporated. The residue is treated with acetic anhydride (10 ml) for 3 h at RT. The mixture is concentrated in vacuo and purified by flash chromatography on silica gel eluting with light petroleum/EtOAc. After re-crystallization from diisopropyl ether the compound (7.1 g) is obtained as a white solid.

1. filtrationAfter completion of the hydrogenation the mixture is filtered
2. customevaporated
3. additionThe residue is treated with acetic anhydride (10 ml) for 3 h at RT
4. concentrationThe mixture is concentrated in vacuo
5. custompurified by flash chromatography on silica gel eluting with light petroleum/EtOAc
6. customAfter re-crystallization from diisopropyl ether the compound (7.1 g)
7. customis obtained as a white solid