反应详情

To a suspension of 5-bromo-1H-isoindole-1,3(2H)-dione (ABCR, 5.0 g) and triphenylphosphine (8.70 g) in tetrahydrofuran (THF) (100 mL) under nitrogen at room temperature was added di-t-butyl azodicarboxylate (7.64 g). The suspension was cooled in an ice/water bath and to this was added iso-propanol (2.032 mL). The reaction mixture was allowed to warm to room temperature to give a pale yellow solution. After 60 minutes, the solvent was removed in vacuo and the residue was dissolved in DCM (30 mL). This was applied to a 750 g silica cartridge and eluted with a gradient of 0-40% ethyl acetate in cyclohexane over 8CV. The required fractions were combined and evaporated in vacuo to give the title compound (5.27 g) as a pale yellow solid.

1. temperatureThe suspension was cooled in an ice/water bath
2. customto give a pale yellow solution
3. customthe solvent was removed in vacuo
4. dissolutionthe residue was dissolved in DCM (30 mL)
5. washeluted with a gradient of 0-40% ethyl acetate in cyclohexane over 8CV
6. customevaporated in vacuo