反应详情

In a 500 mL round bottom flask was charged 1-(3-aminophenyl)pyrrolidin-2-one (5 g, 28.4 mmol), 2,2,10,10-tetramethyl-6-thioxo-3,9-dioxa-5,7-diazaundecane-4,8-dione (9.80 g, 35.5 mmol), polystyrene-carbodiimide (Argonaut P/N 800371, 1.42 mmole/g, 30.0 g, 42.6 mmol) and CH2Cl2 (300 mL). The resulting suspension was stirred at room temperature for 14 hours. The reaction was filtered and the collected solid was washed with 2×30 mL CH2Cl2. The filtrate was concentrated. The concentrate was purified by flash chromatography on a 140 g silica gel plug eluting with CH2Cl2 then 1:1 ethyl acetate/hexanes to provide the title compound. MS (ESI+) m/e 419.1 (M+H)+.

1. filtrationThe reaction was filtered
2. washthe collected solid was washed with 2×30 mL CH2Cl2
3. concentrationThe filtrate was concentrated
4. customThe concentrate was purified by flash chromatography on a 140 g silica gel plug
5. washeluting with CH2Cl2