反应详情

温度

42.5 °C

A 20 L 4-neck round-bottom flask was flushed with N2. Then charged a solution of tert-butyl 2-(1,3-bis(1,3-dioxoisoindolin-2-yl)propan-2-yloxy)ethylcarbamate (919 g, 1.9 mol, 1.0 eq) in ethanol (12000 mL, 13.0 v), followed by dropwise addition of hydrazine hydrate (602 g, 12.0 mol, 6.3 eq) with stirring at 40-45° C. over 30 min. The resulting mixture was stirred for 7 hours at 40-45° C. in an oil bath. The reaction progress was monitored with LCMS. The reaction mixture was cooled to 20˜30° C. and filtered. The filtrate was concentrated under vacuum to give 424.0 g (97.5%) of tert-butyl 2-(1,3-diaminopropan-2-yloxy)ethylcarbamate as a brown oil.

1. customA 20 L 4-neck round-bottom flask was flushed with N2
2. stirringThe resulting mixture was stirred for 7 hours at 40-45° C. in an oil bath
3. temperatureThe reaction mixture was cooled to 20˜30° C.
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under vacuum