Reaktion #94234

Reaktionsgleichung

2-(2-tosyloxyethyl)-1,4-benzodioxan

4-piperidone hydrochloride

sodium carbonate

→

2-[2-(4-oxopiperidino)-ethyl]-1,4-benzodioxan

Lösungsmittel

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe starting material is prepared
2. 2
   FiltrationIt is filtered
3. 3
   Waschenthe residue washed with a small amount of dimethylformamide
4. 4
   Sonstigethe filtrate evaporated
5. 5
   workup.DISSOLUTIONThe residue is dissolved in ethyl acetate
6. 6
   Extraktionthe solution extracted with hydrochloric acid
7. 7
   Temperaturwhile cooling
8. 8
   Extraktionre-extracted with methylene chloride
9. 9
   ExtraktionThe latter extract
10. 10
    Sonstigeis dried
11. 11
    Sonstigeevaporated

Vorschrift

The starting material is prepared as follows: The mixture of 10 g of 2-(2-tosyloxyethyl)-1,4-benzodioxan, 10 g of 4-piperidone hydrochloride, 20 g of anhydrous sodium carbonate and 160 ml of dimethylformamide is stirred vigorously at room temperature for 48 hours. It is filtered, the residue washed with a small amount of dimethylformamide and the filtrate evaporated. The residue is dissolved in ethyl acetate, the solution extracted with hydrochloric acid, the extract made alkaline with 50% aqueous sodium hydroxide while cooling and re-extracted with methylene chloride. The latter extract is dried and evaporated, to yield the 2-[2-(4-oxopiperidino)-ethyl]-1,4-benzodioxan, which solidifies on standing.

Quelle