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. In 5 mL of acetonitrile at room temperature was dissolved 166 mg (1.693 mmol) H2SO4. The solutions were combined resulting in immediate precipitation of a gummy solid. The solid did not redissolve upon reheating, but did triturate into a free-flowing solid. The solids collapsed overnight into a gummy mass which was redissolved in methanol (50 mL) and stripped down to a granular solid which was triturated under acetone (20 mL), filtered, and dried under vacuum at 40 0C resulting in 660 mg (99%). mp 100-105 0C (sharp). 1H NMR (DMSO-dbeta) was consistent with the title salt.Polarized light microscopy revealed the material to be composed of agglomerates of very small crystalline particles. DSC revealed two large and three small endothermic events (Figure 7). Of the two large events, the lower temperature event may correspond to water/solvent loss and the higher temperature event may correspond to melt/decomposition. The three small events may correspond to form changes. DVS revealed that the material is hygroscopic with isotherms characteristic of a weak multi-hydrate (Figure 8). The experiment was terminated near the end of sorption phase of the second cycle. Data from the first cycle indicated that moisture was lost during the desorption phase that had not been lost during the initial drying phase. Approximately 2.5 mole equivalents of water were gained in the first cycle while nearly 4 mole equivalents were gained during the second cycle., 5747-48-8
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Reference£º
Patent; ASTRAZENECA AB; WO2007/62336; (2007); A2;,
Piperazine – Wikipedia
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