Synthetic Route of 13745-86-3, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 13745-86-3, name is 11-Chlorodibenzo[b,f][1,4]thiazepine belongs to chlorides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
EXAMPLE 2Preparation of 11-piperazinyl-Dibenzo[B,F][1,4]Thiazepine,DihydrochlorideDimethylsulfoxide (3.0 L); piperazine (2.45 Kg); toluene (3.0 L) were charged at room temperature under nitrogen and the mixture was heated to 50 C. to 60 C.; stirred at 50 C. to 60 C. till solid dissolves and cooled to 25 C. to 30 C. To it a solution of 11-chloro-dibenzo[b,f]1,4]thiazepine (1.0 Kg) in toluene (6.0 L) was charged at 25 C. to 30 C. and stirred for 3 hours at 25 C. to 30 C. and monitored to completion. The reaction mixture was charged slowly into DI water (45 L) at 25 C. to 30 C. and stirred for 30 minutes at 25 C. to 30 C. The layers were separated at room temperature and the organic layer was washed with DI water (3×3.0 L) at room temperature. The solvent was recovered from the organic layer under vacuum at 50 C. to 55 C. to obtain oil. Ethanol (5 L) was charged into the residue and stirred to dissolve at room temperature. Concentrated hydrochloric acid (0.72 L) was added slowly at 25 C. to 30 C. and stirred until the solid precipitated. The mixture was stirred for 10 hours at 25 C. to 30 C. after precipitation, cooled to 0 C. to 5 C. and stirred for 1 hour at 0 C. to 5 C. The solid was filtered and washed with ethanol (1 L) at 0 C. to 5 C. The solid was added to pre-cooled ethanol (5 L) at 0 C. to 5 C. and stirred for 15 minutes at 0 C. to 5 C. The solid was filtered at 0 C. to 5 C. and washed with ethanol (1 L) at 0 C. to 5 C. The wet cake was unloaded at room temperature under nitrogen atmosphere and dried under vacuum at 55 C. to 60 C. until the moisture content is NMT 5.0% to obtain the title compound.Yield: 1.10 Kg
The synthetic route of 11-Chlorodibenzo[b,f][1,4]thiazepine has been constantly updated, and we look forward to future research findings.
Reference:
Patent; RANBAXY LABORATORIES LIMITED; US2012/71649; (2012); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics