Reaktion #459612

Reaktionsgleichung

sodium iodide

1-[2-chloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-piperazine

3-(2-chloro-ethyl)-2-oxazolidinone

sodium carbonate

→

3-[2-{4-[2-chloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-1-piperazinyl}-ethyl]-2-oxazolidinone

Lösungsmittel

butanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 4 hours together with 8.1 g
2. 2
   SonstigeThen, the solvent is evaporated under reduced pressure
3. 3
   Sonstigethe residue partitioned between water and chloroform
4. 4
   WaschenThe organic phase is washed with water
5. 5
   Trocknendried over sodium sulfate
6. 6
   Sonstigeevaporated under reduced pressure
7. 7
   SonstigeThe residue is recrystallized from methanol

Vorschrift

8.5 G. of 1-[2-chloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-piperazine are stirred at reflux for 4 hours together with 8.1 g. of 3-(2-chloro-ethyl)-2-oxazolidinone, 2.95 g. of sodium carbonate and 0.4 g. of sodium iodide in 50 ml. of butanol. Then, the solvent is evaporated under reduced pressure and the residue partitioned between water and chloroform. The organic phase is washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue is recrystallized from methanol, and there is obtained 3-[2-{4-[2-chloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-1-piperazinyl}-ethyl]-2-oxazolidinone having a melting point of 159°-160° C. The maleate, prepared in acetone, melts at 175°-177° C. (with decomposition). The dihydrochloride hydrate, prepared in ethanol, melts at 179°-181° C. (with decomposition).

Quelle