Реакция #1994244

Уравнение реакции

racemic 2-aminoadipic acid

acetic anhydride

triethylamine

→

N,6-diacetyl-piperidin-2-one

Условия реакции

Обработка

1. 1
   Другоеthe crude reaction product
2. 2
   Концентрированиеis concentrated as
3. 3
   Другоеmuch as possible (rotary evaporator and vane pump)
4. 4
   Промывкаwashed with water (5×20 mL)
5. 5
   ЭкстракцияThe water washings are extracted with CH2Cl2 (2×20 mL)
6. 6
   Концентрированиеconcentrated
7. 7
   ДругоеPurification of 8
8. 8
   ДругоеThe fractions are dried
9. 9
   Концентрированиеconcentrated
10. 10
    Другоеthe product crystallized in the form of pale yellow flakes

Методика

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.

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