Reaktion #953793

Reaktionsgleichung

sodium carbonate

1-[2,8-dichloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-piperazine

propargyl bromide

→

1-[2,8-dichloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-4-(2-propynyl)-piperazine

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture is stirred for 20 hours at room temperature
2. 2
   Sonstigethe solvent is then evaporated under reduced pressure
3. 3
   SonstigeThe residue is partitioned between water and chloroform
4. 4
   SonstigeThe phases are separated
5. 5
   ExtraktionThe aqueous solution is extracted again with chloroform
6. 6
   WaschenThe chloroform solutions are washed with water
7. 7
   Trocknendried over sodium sulfate
8. 8
   Sonstigeevaporated under reduced pressure
9. 9
   SonstigeThe residue is crystallized

Vorschrift

2.87 G. of sodium carbonate are added to a solution of 7.6 g. of 1-[2,8-dichloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-piperazine in 76 ml. of ethanol. Then, a solution of 1.9 ml. of propargyl bromide in 15 ml. of ethanol is added dropwise with stirring. The mixture is stirred for 20 hours at room temperature and the solvent is then evaporated under reduced pressure. The residue is partitioned between water and chloroform. The phases are separated. The aqueous solution is extracted again with chloroform. The chloroform solutions are washed with water, dried over sodium sulfate and evaporated under reduced pressure. The residue is crystallized using diisopropyl ether, and there is obtained 1-[2,8-dichloro-10,11-dihydro-dibenz[b,f]oxepin-10-yl]-4-(2-propynyl)-piperazine having a melting point of 105°-107° C. The dihydrochloride, prepared in ethanol, melts at 213°-215° C. (with decomposition).

Quelle