Reaktion #216260

Reaktionsgleichung

4-piperidone hydrochloride hydrate

4-chlorobenzoyl chloride

potassium carbonate

→

title compound

Ausbeute 74.6%

N-(4-Chlorobenzoyl)-4-piperidone

Ausbeute 74.6%

Lösungsmittel

tetrahydrofuran

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONare added successively
2. 2
   SonstigeThe organic phase is then separated off
3. 3
   Extraktionthe aqueous phase is extracted twice more with ethyl acetate
4. 4
   Sonstigedried
5. 5
   Sonstigeevaporated down
6. 6
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
7. 7
   workup.ADDITIONthe solution is treated with petroleum ether

Vorschrift

87.5 g of 4-chlorobenzoyl chloride and a solution of 276 g of potassium carbonate in 552 ml of water cooled to 5° C. are added successively with stirring to a suspension of 80.6 g of powdered 4-piperidone hydrochloride hydrate in 1 l of tetrahydrofuran. The mixture is stirred at ambient temperature for a further 45 minutes. The organic phase is then separated off, the aqueous phase is extracted twice more with ethyl acetate, and the organic phases are combined, dried and evaporated down. The residue is dissolved in ethyl acetate and the solution is treated with petroleum ether. 88.6 g of the title compound of melting point 61°-63° C. are obtained.

Quelle