反应详情

温度

80 °C

2.29 g (9.6 mmol) of 2-amino-2-(9-fluorenyl)acetic acid, 0.70 g (4.0 mmol) of 4,6-dimethoxy-2-chlorotriazine and 0.51 g (4.8 mmol) of sodium carbonate were introduced into a mixture of 16 ml of DMF and 16 ml of water and stirred at 80° C. for 13 hours. Then ethyl acetate and water were added and the phases were separated. The aqueous phase was acidified with 6 normal HCl and extracted three times with ethyl acetate. The organic phases were dried with MgSO4 and concentrated. The crude product was chromatographed on silica gel with ethyl acetate/n-heptane (1:1). 0.44 g (29.1%) of a white powder was obtained; RF=0.135, melting point 182-186° C.

1. customthe phases were separated
2. extractionextracted three times with ethyl acetate
3. dry with materialThe organic phases were dried with MgSO4
4. concentrationconcentrated
5. customThe crude product was chromatographed on silica gel with ethyl acetate/n-heptane (1:1)