反应详情

A 20 L 4-neck round-bottom flask was flushed with N2. Then charged a solution of 2-(2-(tert-butoxycarbonylamino)ethoxy)propane-1,3-diyl-dimethanesulfonate (929 g, 2.37 mol, 1.0 eq) in N,N-dimethylformamide (9300 mL) and potassium phthalimide (2194 g, 11.85 mol, 5.0 eq). The resulting mixture was stirred for 18 hours at 70˜75° C. in an oil bath. The reaction progress was monitored with LCMS. The reaction mixture was cooled to 20˜30° C., then added icy water (28 L) with stirring. The mixture was stirred for 30 minutes, and then filtered. The filter cake was dried under vacuum at 60° C. to give 919 g (78.5%) tert-butyl 2-(1,3-bis(1,3-dioxoisoindolin-2-yl)propane-2-yloxy)ethylcarbamate as an off-white solid.

1. customA 20 L 4-neck round-bottom flask was flushed with N2
2. temperatureThe reaction mixture was cooled to 20˜30° C.
3. stirringwith stirring
4. stirringThe mixture was stirred for 30 minutes
5. filtrationfiltered
6. customThe filter cake was dried under vacuum at 60° C.