反应详情

温度

60 °C

A 50-mL round bottom flask is charged with racemic 2-aminoadipic acid (2.3 g, 1.43×10−3 mol) and triethylamine (7.5 mL), acetic anhydride (7.5 mL), and a catalytic amount of DMAP (15 mg). The mixture is heated to 60° C. for 24 h; the progress of the reaction is followed by TLC (eluent: ethyl acetate/petroleum ether, 8/2). Once the reaction is complete, the crude reaction product is concentrated as much as possible (rotary evaporator and vane pump) and then washed with water (5×20 mL). The water washings are extracted with CH2Cl2 (2×20 mL). The organic layers are combined and concentrated. Purification of 8 is carried out on a silica gel column (eluent: ethyl acetate/petroleum ether, 8/2). The fractions are dried, concentrated and the product crystallized in the form of pale yellow flakes.

1. customthe crude reaction product
2. concentrationis concentrated as
3. custommuch as possible (rotary evaporator and vane pump)
4. washwashed with water (5×20 mL)
5. extractionThe water washings are extracted with CH2Cl2 (2×20 mL)
6. concentrationconcentrated
7. customPurification of 8
8. customThe fractions are dried
9. concentrationconcentrated
10. customthe product crystallized in the form of pale yellow flakes