Category: piperazines

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.

In 5 mL of acetonitrile was dissolved 500 mg (1.693 mmol) of 11-piperazin-l- yldibenzo[b,f][l,4]thiazepine. In 5 mL of acetonitrile was dissolved 197 mg fumaric acid (1.693 mmol) with heating. The solutions were combined resulting in precipitation. The solid redissolved upon heating and then crystallized more slowly upon cooling, generating a free- flowing solid. The mixture did not change overnight. The solids were collected, washed with acetonitrile (5 mL), and dried under vacuum at 400C resulting in 574 mg (82.3%) of crystalline solid, mp 159-163 0C (dec). 1H NMR (DMSOd6) was consistent with the title salt.Polarized light microscopy revealed the rod-shaped crystalline particles. DSC revealed one endotherm at 153.3 0C which appeared to be a melt event preceding eventual decomposition at higher temperatures (Figure 3). TGA revealed 1.4% weight loss in the water/solvent temperature region (Figure 3). DVS indicated that the salt was hygroscopic with isotherms characteristic of hydrate formation (Figure 4). The sorption isotherms of each cycle were different, indicating possible form change. The plateau of the first cycle (diamond) between 50 and 80% RH was about equal to 1 mole equivalent of water. The plateau in the same region of the second cycle (triangle) was equal to about 2.5 mole equivalents gained from the starting point of the second cycle at 0% RH. The observation that the second cycle started at a lower mass than the first cycle was probably due to incomplete drying of the sample prior to the cycling.

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

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.5625-67-2,Piperazin-2-one,as a common compound, the synthetic route is as follows.

Piperazine-2-one (1 g, 10 mmol) is added to ethyl acetate (40 mL),In the solution of 20 ml ,K2CO3 is added at the room temperature followed by Benzyloxycarbonyl chloride (2.1 mL, 15 mmol) is added dropwise to the reaction flask,and reaction is stirred at room temperature . The reaction stopped next day, and the organic layer is washed with 20 mL of X saturated NaCl solution, dried over anhydrous magnesium sulfate,Column chromatography (D: Mu = 75: 1) to obtain a white solid 1.48, 59.8%.yield.

5625-67-2, As the paragraph descriping shows that 5625-67-2 is playing an increasingly important role.

Reference：
Patent; Chinese Academy Of Medical Sciences Pharmaceutical Institute; Xu Boling; Chen Xiaoguang; Zhou Jie; Ji Ming; Yao Haiping; Zhou Qin; (57 pag.)CN107098886; (2017); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

21043-40-3, 1-Cyclopentylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of [2-(4-methyl-naphthalen-1-yl)-3H-imidazol-4-yl]-methanol (50 mg, 0.21 mmol) in 1 ,2-dichloroethane (5 ml) at 0C is added thionylchloride (5 eq.). The resulting mixture is stirred at 50C for 1 hr. Solvent and remaining thionylchloride are evaporated, and the residue is dissolved in acetonitrile (3 ml), followed by the addition of substituted 4-cyclopentylpiperazine (1.0 eq.) and potassium carbonate (2.0 eq.). The resulting mixture is stirred at rt overnight. The reaction is diluted with EtOAc (10 ml), washed with brine, dried, and solvent is removed. The crude product is purified through PTLC to give l-cyclopentyl-4-[2-(4-methyl-naphthalen-1-yl)-3H-imidazol-4- ylmethyl]-piperazine. LCMS 375 (M+ +1).

21043-40-3, As the paragraph descriping shows that 21043-40-3 is playing an increasingly important role.

Reference：
Patent; NEUROGEN CORPORATION; WO2006/89076; (2006); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

314741-40-7, (S)-tert-Butyl 3-(hydroxymethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

60% Sodium hydride (60 mg, 1.49 mmol) was added to a suspension of te/t-butyl (S)-3- (hydroxymethyl)piperazine-l-carboxylate (161 mg, 0.75 mmol) and 7-bromo-6-chloro-5-fluoro-2- morpholinoquinazolin-4(3/-/)-one (208 mg, 0.57 mmol) in THF (10 ml) at 0C under nitrogen and stirred for 5 minutes. The reaction mixture was allowed to warm to room temperature then stirred at 65C for 1 hour, allowed to cool, then quenched at 0C with acetic acid (0.1 ml). The reaction mixture was diluted with ethyl acetate (50 ml), washed with aqueous 2M potassium carbonate solution (10 ml) then dried (MgS04) and the solvent evaporated. The residue was purified by flash silica chromatography, elution gradient 0 to 10% 2N methanolic ammonia in DCM. Pure fractions were evaporated to dryness to afford te/t-butyl (S)-3-(((7-bromo-6-chloro-2-morpholino-4-oxo-3,4-dihydroquinazolin-5- yl)oxy)methyl)piperazine-l-carboxylate (215 mg, 67%) as a white foam, m/z: ES+ [M+H]+ 558 / 560., 314741-40-7

The synthetic route of 314741-40-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ASTRAZENECA AB; KETTLE, Jason, Grant; BAGAL, Sharanjeet, Kaur; BOYD, Scott; EATHERTON, Andrew, John; FILLERY, Shaun, Michael; ROBB, Graeme, Richard; RAUBO, Piotr, Antoni; (144 pag.)WO2018/206539; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

848482-93-9,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.848482-93-9,(S)-4-(tert-Butoxycarbonyl)piperazine-2-carboxylic acid,as a common compound, the synthetic route is as follows.

(S)-4-Boc-2-piperazinecarboxylic acid (530 mg, 2.17 mmol) was dissolved in MeOH (25 mL) and formaldehyde (1.76 mL, 37 wt % in water, 21.7 mmol) was added. The reaction mixture was stirred for 30 min, NaBH(OAc)3 (0.92 g, 4.34 mmol) was added and the reaction mixture was stirred for 2 h. The solvents were removed in vacuo and the residue was purified by reverse phase column chromatography. The residue and benzyl homopiperazine (0.41 g, 2.17 mmol) were dissolved in DMF (20 mL) and cooled to 0 C. DIPEA (0.59 g, 4.56 mmol) and HBTU (0.82 g, 2.17 mmol) were added and the reaction mixture was stirred for 3 h. The solvents were removed in vacuo and the residue was partitioned between DCM (100 mL) and water (50 mL). The organic fraction was washed with 1M aq Na2CO3 (25 mL), brine (25 mL), dried (MgSO4) and concentrated in vacuo. The residue was purified by reverse phase column chromatography to give the title compound (0.64 g, 71%) as a light yellow gum. LCMS (ES+): 417.4 [MH]+.

The synthetic route of 848482-93-9 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Proximagen Limited; Savory, Edward Daniel; Stewart, Allson; Cartey, Allison; Brown, Giles; Simpson, Iain; Oliver, Kathryn; Patient, Lee; Higginbottom, Michael; Cole, Andrew Graham; US2013/289020; (2013); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

154590-35-9, tert-Butyl 4-(4-amino-2-fluorophenyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step B. 4-[4-(2-Ethyl-butyrylamino)-2-fluoro-phenvH-piperazine-1-carboxylic acid tert-butyl ester. 4-(4-Amino-2-fluoro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester(4.54 g, 15.4 mmol) and DIPEA (2.95 ml_, 16.9 mmol) were dissolved in DCM (90.0 ml.) and cooled to 00C. 2-Ethyl-butyryl chloride (2.28 ml_, 16.2 mmol) was added slowly. The resulting mixture was then stirred at 00C for 1 h and at room temperature for 4 h. The resulting mixture was then washed with water, 1 N NaOH solution and water. The organic phase was dried (Na2SO4), filtered and concentrated to yield a residue. Chromatography of the residue (SiO2, 0-8 % acetone/DCM) yielded the title compound.MS (ESI) mass calculated for C21H32FN3O3, 393.50, m/z measured, 394.6 [M+H]+ 1H NMR (CDCI3): 7.50 (dd, J = 13.9, 2.4, 1 H), 7.22 (s, 1 H), 7.15-7.07 (m,1 H), 6.88 (t, J = 9.0, 1 H), 3.63-3.52 (m, 4H), 3.00-2.92 (m, 4H), 2.06-1.93 (m, 1 H), 1.75-1.65 (m, 2H), 1.59-1.52 (m, 2H), 1.48 (s, 9H), 1.00-0.88 (m, 6H)., 154590-35-9

As the paragraph descriping shows that 154590-35-9 is playing an increasingly important role.

Reference：
Patent; JANSSEN PHARMACEUTICA N.V.; WO2009/79597; (2009); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5317-33-9, 3-(4-Methylpiperazin-1-yl)propan-1-ol is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,5317-33-9

The 4-CHLORO-3-CYANO-6-METHOXY-7- [3- (4-METHYLPIPERAZIN-1-YL) PROPOXY] QUINOLINE used as a starting material was prepared as follows:- A mixture of 3-bromopropanol (20 ml), N-METHYLPIPERAZINE (29 ml), potassium carbonate (83 g) and ethanol (200 ml) was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70C under about 0.2 mm Hg to give 1- (3-HYDROXYPROPYL)-4-METHYLPIPERAZINE (17 g); NMR Spectrum : (CDC13) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2. 8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H). A solution OF DIISOPROPYL AZODICARBOXYLATE (12.1 ml) in methylene chloride (50 ml) was added dropwise during 30 minutes to a stirred mixture OF 4-CHLORO-3-CYANO-7-HYDROXY- 6-methoxyquinoline (12 g), 1- (3-HYDROXYPROPYL)-4-METHYLPIPERAZINE (9.7 g), triphenylphosphine (16.1 g) and methylene chloride (200 ml) that had been cooled to 5C. The resultant mixture was allowed to warm to ambient temperature and was then stirred for 1 hour. Further portions of diisopropyl azodicarboxylate (1.2 ml) and triphenylphosphine (1.6 g) were added and the mixture was stirred at ambient temperature for a further 1 hour. The mixture was poured into water and the organic layer was separated, washed with a saturated brine solution, dried over magnesium sulphate and evaporated. The material so obtained was purified by column chromatography on silica using increasingly polar mixtures of methylene chloride and methanol as eluent. There was thus obtained the required starting material as a solid (14.5 g); NMR Spectrum : (DMSOd6) 1.95 (m, 2H), 2.13 (s, 3H), 2.24-2. 5 (m, 10H), 4.0 (s, 3H), 4.25 (t, 2H), 7.43 (s, 1H), 7.51 (s, 1H), 8.95 (s, 1H) ; Mass Spectrum : MASS 375 and 377.

5317-33-9 3-(4-Methylpiperazin-1-yl)propan-1-ol 79208, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/41811; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

21655-48-1, cis-2,6-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Preparation 3: 1-[4-((3R,5S)-3,4,5-trimethyI-piperazin-1-yI)-phenyI]-ethanone; STEP A; A mixture of 4-fluoro-benzonitrile (1.12 g, 9.25 mmol), (2R,6S)-2,6-dimethyl- piperazine (1.58 g, 13.9 mmol) and K2CO3 (3.20 g, 23.12 mmol) in DMSO (50 ml) was stirred at 1300C for 24 h. The mixture was then partitioned between water and AcOEt and the organic phase was washed twice with water. The organic layer was then dried over Na2SO4 and evaporated in vacuo. The residue was taken up with Et2O, treated with HCI/Et2O and the resulting precipitate was filtered to give 2.2 g of 4-((3R,5S)-3I5-dimethyl-piperazin-1-yl)-benzonitrile hydrochloride as a yellow powder. Y= 94percent, 21655-48-1

As the paragraph descriping shows that 21655-48-1 is playing an increasingly important role.

Reference：
Patent; DAC S.R.L.; WO2007/113249; (2007); A2;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.59878-57-8,1-(Cyclopropylcarbonyl)piperazine,as a common compound, the synthetic route is as follows.

100 mg (0.32 mmol) of 5,5′-diallyl-3- (chloromethyl)-[1,1′-biphenyl] -2,2′-diol (Intermediate 4),59mg (0.38mmol) 1-cyclopropanoylpiperazine,140.44mg (0.43mmol) of cesium carbonate, a catalytic amount of potassium iodide was added to a 10ml round bottom flask, acetonitrile was added to dissolve, heated to 80 C, and reacted overnight. After the reaction was completed, the reaction solution was cooled to room temperature, and then poured into water. It was extracted with ethyl acetate, washed with saturated brine, dried over anhydrous sodium sulfate, spin-dried, and passed through a column (dichloromethane-methanol = 20/1) to obtain 98 mg of an off-white powdery solid with a yield of 70.9%., 59878-57-8

As the paragraph descriping shows that 59878-57-8 is playing an increasingly important role.

Reference：
Patent; Sichuan University; Chen Lijuan; Wei Yuquan; Ye Haoyu; (42 pag.)CN110343033; (2019); A;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.31166-44-6,1-Cbz-Piperazine,as a common compound, the synthetic route is as follows.

To a solution of propylene oxide (4.0 mL, 57 mmol) in DCM (160 mL) was added 2.0M of trimethylaluminum in toluene (27 mL, 54 mmol) at -78 °C under N2. After being stirred at that temperature for 10 min, a solution of benzyl piperazine-l-carboxylate (from Aldrich, 9 mL, 40 mmol) in DCM (60 mL) was added. The resulting reaction mixture was stirred at -78 °C for 30 min. The reaction was then allowed to warm up to 0 °C, stirring for another 30 min. To the reaction mixture was added sodium fluoride (8.2 g, 200 mmol) in one portion, followed by water (5.2 mL, 290 mmol) slowly and periodically at 0 °C. The resulting suspension was rapidly stirred for 1 h at 0 °C and filtered through a short column of Celite and the column was subsequently washed with DCM (120 mL). The combined filtrates were dried over Na2S04, concentrated and purified on silica gel (eluting with 0-10percent MeOH in DCM) to provide the desired product (9.6 g, 76percent). LCMS calculated forCi5H23 203(M+H)+: m/z = 279.2; Found: 279.3. 3/4 NMR (500 MHz, DMSO-d6): delta 7.39-7.31 (5H, m), 8.07 (2H, s), 4.29 (1H, J= 4.0 Hz), 3.75 (1H, m), 3.38 (4H, br s), 2.38 (4H, m), 2.24 (1H, dd, J= 12.5 and 7.0 Hz), 2.17 (1H, dd, J= 12.5 and 7.0 Hz), 1.04 (3H, d, J= 6.0 Hz) ppm.

31166-44-6, As the paragraph descriping shows that 31166-44-6 is playing an increasingly important role.

Reference：
Patent; INCYTE CORPORATION; RODGERS, James, D.; LI, Yun-Long; SHEPARD, Stacey; WANG, Haisheng; WO2011/28685; (2011); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics