Category: 5747-48-8piperazines

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5747-48-8,11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine,as a common compound, the synthetic route is as follows.

5747-48-8, A 1 liter round bottom flask equipped with stirring rod, thermo pocket, water condenser was charged with solution of l l-piperazinyldibenzo[b,fj [l,4]thiazepine in toluene 350 cc [63.0 g (0.22 moles)] and the mixture was stirred for 15 min 25- 30C, to which, was added sodium carbonate [41.0 gm (0.39 moles)], tetra butyl ammonium bromide [16.0 gm (0.05 mole)] and 2-(2-chloroethoxy) ethanol [32.0 gm ( 0.257 moles)] at room temperature. The reaction mixture was heated to reflux at 110- 112C. The reaction mixture was maintained at reflux for 10-12 hrs. The reaction mixture was analyzed by HPLC (to check for absence of compound IV) and was cooled to at 25C to 30C,and was added 150 cc DM water, the reaction mixture was stirred for 30 min at 25-30C. The layers were separated and the aqueous layer extracted with 50 cc toluene. The extract and the organic layer were combined, and the pH was adjusted to 2-3 using IN HCl solution in DM water, the reaction mixture was stirred for 30 min at 25-3O0C. The layers were separated and the aqueous layer washed with 100 cc toluene twice. To the aqueous layer was added 250 cc toluene, and the pH was adjusted to 8-10 using sodium carbonate, the reaction mixture was stirred for 30 min at 25-30C. The layers were separated and the aqueous layer extract with 125 cc toluene. The extract and the organic layer were combined, and washed with DM water 300 cc twice. The organic layer was distilled off under vacuum below 500C leaving 50-60 cc toluene with product. Purity of 2-(2-(4- dibenzo[b,f]-[l,4] thiazepine- l l-yl-l-piperazinyl)ethoxy) ethanol in toluene was 99.0% (area % by HPLC). To this solution 1000 cc absolute ethanol was added with activated carbon 5.0 gm and heated to reflux for 90 min. The resulting solution was cooled to 50-550C and filtered. The resulting solution was added 12.5 gm (0.5 moles) fumaric acid at 500C. The reaction mixture was heated to reflux for 2 hrs and was slowly cooled to room temperature and maintained for 2 hrs at room temperature. The reaction mass was filtered and washed with 200 cc absolute ethanol. The wet material obtained was dried under vacuum at 50-55C to afford quetiapine fumarate. Dry weight of quetiapine fumarate is 60-65 gm. Purity of quetiapine fumarate was 99.5% (area % by HPLC).

As the paragraph descriping shows that 5747-48-8 is playing an increasingly important role.

Reference£º
Patent; TEVA PHARMACEUTICAL INDUSTRIES LTD.; TEVA PHARMACEUTICALS USA, INC.; WO2008/121415; (2008); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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 2; In a reaction vessel, a mixture of 1 l-piperazinyldibenzo[b,fj[l,4]-thiazepine ( 10 Kg), 2- (2-chloroethoxy)ethanol (6.33 kg), sodium carbonate (21.55 kg), 1 kg tetrabutyl ammonium bromide and 0.2 kg sodium iodide was heated in 30 liters of water to about 100 0C. The reaction mixture was maintained at about 100 to 1050C for about 5 hours. EPO Starting l l-piperazinyldibenzo[b,f][l,4]-thiazepine was about 0.3 % by HPLC. Maintained for another 2 hours till the l l-piperazinyldibenzo[b,f][l,4]-thiazepme was about less than 0.08 % by HPLC analysis. The reaction mass was cooled to about 30 0C and aqueous layer extracted with methylenedichloride(100 liters). The organic layer was washed with water and concentrated under reduced pressure. The oily residue was so obtained was suspended in 100 litres of ethanol ( commercial) and 4.1 kg fumaric acid was added. The mixture was stirred for about 4 hours and cooled to about 1O0C. The precipitated quetiapine hemi-fumarate salt was filtered and dried to give 12Kg ( yield 80 % & purity 99.8% by HPLC analysis), 5747-48-8

Big data shows that 5747-48-8 is playing an increasingly important role.

Reference£º
Patent; IPCA LABORATORIES LIMITED; WO2006/77602; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5747-48-8,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5747-48-8,11-(Piperazin-1-yl)dibenzo[b,f][1,4]thiazepine,as a common compound, the synthetic route is as follows.

General procedure: To a solution of isocyanate (1.877mmol) in toluene (2.5mL) was added a solution of a monosubstituted piperazine (1.877mmol) in toluene (1.0mL). The reaction mixture was heated at 40-45C for 30 to 60min. The reaction mixture was then cooled down to room temperature (22-25C) and the resulting solids were filtered and washed with more toluene (2.0mL). The wet solids were then placed in 2.0mL of toluene, stirred at room temperature for about 30min, filtered and washed with toluene (1.0mL) to obtain the crude disubstituted piperazine derivative. Finally, all crude derivatives were purified by silica-gel column chromatography using a mixture of dichloromethane/methanol (9:1) to afford pure piperazines products.

As the paragraph descriping shows that 5747-48-8 is playing an increasingly important role.

Reference£º
Article; Patil, Mahadev; Noonikara Poyil, Anurag; Joshi, Shrinivas D.; Patil, Shivaputra A.; Patil, Siddappa A.; Bugarin, Alejandro; Bioorganic Chemistry; vol. 92; (2019);,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics