反応 #2028939

反応方程式

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

→

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

溶媒

toluene

反応条件

後処理

1. 1
   その他evaporated to dryness on a rotary evaporator
2. 2
   workup.ADDITIONThe resulting hard solid was then charged to a jacketed vessel
3. 3
   温度cooled to 5° C.
4. 4
   workup.WAITheld for 4 h

実験手順

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.

出典