Reaktion #2028939

Reaktionsgleichung

11-piperazin-1-yldibenzo[b,f][1,4]thiazepine hydrochloride

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11-piperazin-1-yldibenzo[b,f][1,4]thiazepine

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeevaporated to dryness on a rotary evaporator
2. 2
   workup.ADDITIONThe resulting hard solid was then charged to a jacketed vessel
3. 3
   Temperaturcooled to 5° C.
4. 4
   workup.WAITheld for 4 h

Vorschrift

The above procedure was repeated for an additional four aqueous solutions of 11-piperazin-1-yldibenzo[b,f][1,4]thiazepine hydrochloride and the five resulting toluene solutions were combined and evaporated to dryness on a rotary evaporator. The resulting hard solid was then charged to a jacketed vessel and slurried with methyl-t-butyl ether (MTBE) (500 mL). The resulting slurry was stirred overnight at ambient temperature and then cooled to 5° C. and held for 4 h. The solid 11-piperazin-1-yldibenzo[b,f][1,4]thiazepine product was isolated on a no. 3 sinter and washed with 200 mL of cold MTBE. The cake was dried in a vacuum oven overnight at 60° C. yielding 373 g of product.

Quelle