5747-48-8, 11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
EXAMPLE 5; Preparation of Quetiapine from ll-piperazinyldibenzo[b,f][l,4]thiazepine; [0040] 33.1 g of extra fine potassium carbonate is added to the r¡ã-butanol solution of 1 l-piperazinyldibenzo[b,fj[l54]thiazepine with continuous stirring. Then, 16.48 g of sodium iodide and 35.97 g of 2-(2-chloroethoxy)ethanol are respectively added with stirring. With continued mixing, the reaction mixture is heated to a temperature of 102 C and maintained at that temperature for 12 – 16 hours. The conversion of 11- piperazinyldibenzo[b,fj[l,4]thiazepine to quetiapine can be monitored by HPLC analysis. Once the conversion of is complete, the reaction mixture is cooled to a temperature of less than about 80 0C and about 500 g of water is added to adjust the reaction mixture to a temperature of about 40 – 50 C and the mixing is continued for at least about 30 minutes. The biphasic mixture is transferred to a separatory funnel and the aqueous and organic phases are allowed to separate. The lower aqueous phase is isolated and discarded. The upper organic phase containing crude quetiapine is transferred to a flask. Another 25O g of water is added to the quetiapine solution and the reaction mixture is stirred at a temperature of about 40 – 50 C for at least 30 additional minutes. The biphasic mixture is again transferred to a separatory funnel and the aqueous and organic phases are allowed to separate. The lower aqueous phase is removed and discarded. The upper organic phase containing crude quetiapine is recovered and transferred to a flask and distillation setup suitable for vacuum distillation to azeotropically remove water. Vacuum is applied to the distillation setup as the solution is heated, possibly to a temperature as high as 55 – 65 C at the end of the distillation, to remove water. The distillation is continued until no more water is observed collecting in the collection trap. The still bottoms may be checked by KF moisture analysis; the amount of KF water should be less than 0.5% by weight. Once the distillation is complete, the crude quetiapine solution is cooled to a temperature of less than 30 0C., 5747-48-8
The synthetic route of 5747-48-8 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; CAMBREX CHARLES CITY, INC.; WO2006/135544; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics