Analyzing the synthesis route of 5747-48-8

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

In 5 mL of acetonitrile was dissolved 500 mg (1.693 mmol) of 11-piperazin-l- yldibenzo[b,fj[l,4]thiazepine. Ih 5 mL of acetonitrile was dissolved 254 mg (1.693 mmol) of L- tartaric acid with heating. The solutions were combined and a slightly gummy solid precipitated immediately. The mixture was diluted with an additional 5 mL of acetonitrile. The solid did not dissolve, but triturated into a free-flowing solid. The mixture did not change overnight. The solids were collected, washed with acetonitrile (5 mL), and dried under vacuum at 40 0C resulting in 707 mg crystalline solid (93.8%). mp 170-175 0C (dec). 1H NMR (DMSOd6) was consistent with the title salt.Polarized light microscopy showed that the solid was composed of irregularly shaped crystalline particles. DSC revealed two broad endotherms at 118.3 and 175.1 0C (Figure 1). The lower temperature endothermic event is likely due to water loss and the higher temperature endothermic event may be due to a melt followed by decomposition. TGA revealed two weight loss transitions (Figure 1). The lower temperature weight loss transition coincided with the lower temperature DSC event and was measured to correspond to approximately 1 mole equivalent of water. The higher weight loss transition coincided with the higher DSC event. Dynamic vapor sorption (DVS) studies indicated that the salt was hygroscopic (Figure 2). Moisture gain was reversible with little hysteresis and amounts to about 1 mole equivalent at 90% RH which was in addition to the moisture already contained in the salt., 5747-48-8

The synthetic route of 5747-48-8 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; WO2007/62336; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics