Reaktion #522784

ord-10e8acb73da7461f9aed86261adb2eb8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe mixture is heated for 24 hours
  2. 2
    Temperaturunder reflux
  3. 3
    Waschenthe organic phase washed with saturated soda solution and water
  4. 4
    Trocknendried over sodium sulphate
  5. 5
    Einengenconcentrated under reduced pressure

Vorschrift

2.7 g of 1-(10,11-dihydro-2-methyl-dibenzo[b,f]thiepin--10-yl)-piperazine are treated, together with 4.3 g of powdered potassium carbonate, 200 mg of potassium iodide and 90 ml of toluene, with 3.2 g of N-(β-chloroethyl-oxazolidinone and the mixture is heated for 24 hours under reflux. Then the mixture is poured on to ice-water, diluted with benzene and the organic phase washed with saturated soda solution and water, dried over sodium sulphate and concentrated under reduced pressure. There is obtained 3-[2-[4-(10,11-dihydro--2-methyl-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl]--2-oxazolidinone which is recrystallised from acetone/petroleum ether. The maleate melts at 159°-161° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04006145uspto-grants-1977_02