反应详情

A solution of {2-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-vinyl]-phenyl}-acetic acid tert-butyl ester (1.97 g) and hydrazine hydrate (1.97 mL) in EtOH (75 mL) was heated at reflux for 90 minutes. The solids were removed by filtration and the filtrate was concentrated in vacuo. The residue was dissolved in EtOAc (50 mL) and the solution was washed with saturated NaHCO3 followed by brine. The organic solution was dried over MgSO4, filtered, and concentrated. Purification by flash chromatography (CHCl3:MeOH 97.5:2.5 to 95:5 to 9:1) provided the title amine (853 mg). MS 236 (M+1).

1. temperatureat reflux for 90 minutes
2. customThe solids were removed by filtration
3. concentrationthe filtrate was concentrated in vacuo
4. dissolutionThe residue was dissolved in EtOAc (50 mL)
5. washthe solution was washed with saturated NaHCO3
6. dry with materialThe organic solution was dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated
9. customPurification by flash chromatography (CHCl3:MeOH 97.5:2.5 to 95:5 to 9:1)