Reaktion #1994243

Reaktionsgleichung

Compound 5

N,5-diacetylpyrrolidin-2-one

K2CO3

hydrochloric acid

→

Compound 6

Ausbeute 48.0%

5-acetylpyrrolidin-2-one

Ausbeute 48.0%

Lösungsmittel

ethyl acetate methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring for 3.5 hrs
2. 2
   Sonstigefreeze-dried for 16 hrs
3. 3
   ExtraktionThe organic residue is then extracted with CH2Cl2 (40 mL)
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated under reduced pressure
6. 6
   Sonstigeto provide a brown viscous liquid
7. 7
   SonstigePurification

Vorschrift

In a round bottom flask, Compound 5 (2.2 g, 13×10−3 mol) is treated with a solution of K2CO3 (5.6 g, 40×10−3 mol, in 20 mL of water), with magnetic stirring at room temperature. The progress of the reaction is followed by TLC (eluent: ethyl acetate/methanol, 98/2). After stirring for 3.5 hrs, the reaction is complete. The reaction mixture is neutralized (pH=7) by adding 1N hydrochloric acid and then freeze-dried for 16 hrs. The organic residue is then extracted with CH2Cl2 (40 mL), filtered and then concentrated under reduced pressure to provide a brown viscous liquid. Purification was carried out on a silica gel column (eluent: ethyl acetate/methanol, 98/2). Compound 6 is obtained after such purification as a white powder.

Quelle