Month: September 2021

55276-43-2,55276-43-2, 1-Methanesulfonylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

(S)-Epichlorohydrin (48.0 mL, 0.612 mol) was added to a stirred solution of piperazine N-methylsulfonamide (87.3 g, 0.532 mol) in ethanol (1.33 L) at room temperature. The reaction mixture was stirred for 18 h and the white solid precipitate which formed was collected by filtration and washed with ethanol to provide the title intermediate (107.7 g) as a white solid which was used without further purification. (m/z): [M+H]+ calcd for C8H17ClN2O3S, 257.07; found, 257.2. 1H-NMR (DMSO): delta(ppm) 5.09 (d, 1H), 3.84 (m, 1H), 3.65 (dd, 1H), 3.55 (dd, 1H), 3.09 (m, 4H), 2.37 (dd, 1H), 2.86 (s, 3H), 2.50-2.58 (m, 4H), 2.45 (dd, 1H).

55276-43-2 1-Methanesulfonylpiperazine 709161, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Theravance, Inc.; US2006/276482; (2006); A1;,
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.109-07-9,2-Methylpiperazine,as a common compound, the synthetic route is as follows.

109-07-9, {4- [5-BROMOTHIOPHEN-2-YL]-PYRIMIDIN-2-YL}- (2, 2,6, 6-TETRAMETHYL-PIPERIDIN-4-YL)-AMINE, (Step C of Example 5,395 mg, 1 MMOL), Pd (OAC) 2 (20 mg), R- (+)-BINAP (20 mg), 2- methylpiperazine (500 mg, 5 mmol) and NaOtBu (400 mg, 4 mmol) were dissolved in 1,4- dioxan (6 ml) and refluxed for 3 hours. The reaction mixture was poured on water and extracted 3 times with EtOAc. The combined organic phases were dried over sodium sulfate, filtered through a bed of silicagel (TBME/MeOH/ammonia : 90/10/1) and purified via preparative HPLC to give the title compound as yellow crystals. Yield: 10 mg (2%). MS (ESI): 415 [M+H] + LH-NMR (CDCI3) : No. (ppm) 8.12 (d, 1H), 7.43 (d, 1 H), 6.73 (d, 1H), 6.10 (d, 1H), 4. 88 (br d, 1 H), 4.45 (m, 1H), 3.48 (br d, 2H), 2.90-3. 17 (M, 5H), 2.59 (br t, 1H), 2.13 (br d, 2H), 1.41-1. 79 (m, 14H), 1.18 (d, 3H).

As the paragraph descriping shows that 109-07-9 is playing an increasingly important role.

Reference：
Patent; NOVARTIS AG; NOVARTIS PHARMA GMHBH; WO2004/89913; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

196811-66-2, tert-Butyl 4-carbamothioylpiperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

The production of compound No. 49 proceeds according to the sequence of reaction steps shown in the following scheme: The initial step is as described in example 14. Then the conversion from 5 to 25 was performed during 6 hours at reflux in methanol in the presence of a molar equivalent of 24 and a molar equivalent of sodium hydrogenocarbonate, and the desired intermediate 25 was obtained in 81% yield. The conversion from 25 to 26 was performed during 3 hours at 20 C. in the presence of triethylamine, and the desired intermediate 26 was obtained in 73% yield. The conversion from 26 to the final compound No. 49 was performed during 6 hours at 20 C. in the presence of a molar excess of triethylamine., 196811-66-2

As the paragraph descriping shows that 196811-66-2 is playing an increasingly important role.

Reference：
Patent; NV reMYND; US2010/197703; (2010); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

25057-77-6, 1,2-Dimethylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Reference Example 7 To a solution of N-benzyl-4-piperidone (8.0 g) and 3,4-dimethylpiperazine (9.5 g) in ethanol (100 ml) are added 5% platinum-carbon (2 g) and acetic acid (14.4 ml), and the mixture is subjected to catalytic hydrogenation at room temperature under atmospheric pressure. The catalyst is removed by filtration, and the filtrate is concentrated under reduced pressure. Water is added to the resultant, and the mixture is basified with a 5% aqueous sodium hydroxide solution, and the mixture is extracted with diethyl ether. The extract is washed with water, dried and concentrated under reduced pressure to remove the solvent. The residue is dissolved in ethanol, and thereto is added to conc. hydrochloric acid to give a hydrochloride. The resulting white powder is collected by filtration, dissolved in water, and basified with a 5% aqueous sodium hydroxide solution. The mixture is extracted with diethyl ether, washed with water, dried, and concentrated under reduced pressure to give 4-(3,4-dimethyl-1-piperazinyl)-1-benzylpiperidine (4.2 g). 1 H-NMR (CDCl3) deltappm: 1.04 (3H, d, J=6 Hz), 1.45-2.5 (12H, m), 2.27 (3H, s), 2.7-3.05 (4H, m), 3.48 (2H, s), 7.31 (5H, m).

25057-77-6, The synthetic route of 25057-77-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Otsuka Pharmaceutical Company, Limited; US6140330; (2000); 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.59702-07-7,1-Methylpiperazin-2-one,as a common compound, the synthetic route is as follows.

59702-07-7, EXAMPLE 18 4-Methyl-3-oxo-piperazine-1-carboxylic Acid (4-methoxy-7-piperidin-1-yl-benzothiazol-2-yl)-amide Using 4-methoxy-7-piperidin-1-yl-benzothiazol-2-ylamine and 4-methyl-3-oxo-piperazine, the title compound was prepared as yellow solid in 84percent yield. MS: m/e=404(M+H+).

The synthetic route of 59702-07-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Flohr, Alexander; Jakob-Roetne, Roland; Norcross, Roger D.; Riemer, Claus; US2003/149036; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

5464-12-0, 1-(2-Hydroxyethyl)-4-methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

5464-12-0, PPh3 (0.0325 mol) was added dropwise at a temperature between 0 and [5°C] to a solution of Vanillin (CA No : [121-33-5)] (0. [025 MOL),] intermediate 14 (0.03 mol) and DIAD (0.0375 mol) in THF (60ml). The mixture was stirred at room temperature for 18 hours. EtOAc was added. The mixture was extracted twice with [HC13N.] The acidic layer was washed with EtOAc, basified with [K,, C03] and extracted with EtOAc. The organic layer was dried [(MGS04),] filtered, and the solvent was evaporated. Yielding: 3.9g of intermediate 15 [(56percent).

As the paragraph descriping shows that 5464-12-0 is playing an increasingly important role.

Reference：
Patent; JANSSEN PHARMACEUTICA N.V.; WO2004/7498; (2004); 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.75336-86-6,(R)-2-Methylpiperazine,as a common compound, the synthetic route is as follows.

75336-86-6, To the 1200 L reactor was dissolved (R)-2-methylpiperazine from Example 5 (25 kg) in CH3CN (319 kg) at [15°C] to [25°C] until dissolution was complete (10 min. ) After cooling to [5°C] to [10°C] Et3N (63 kg) was added. To the 1200 L receiver trityl chloride (69.5 kg) was dissolved in CH2C12 (106 kg) at [15°C] to [25°C.] The solution in the receiver was transferred to the reactor over 0.5 h with a CH2C12 rinse (27 kg), and the solution was heated to [20°C] to [30°C.] The reaction was monitored by GLC and was complete in 1 h. The resulting slurry was cooled to [8°C] to [12°C,] filtered onto a 48″Nutsche filter, and rinsed with CH3CN (40 kg at [8°C] to [12°C).] The filter cake was dried using [50°C] to [55°C] nitrogen to afford 25.26 kg of the by-product [ET3NHCL] (74percent yield; easy to filter off the by-product). The filtrate was transferred to the 1200 L reactor and cooled further [TO-8°C] [TO-10°C] for 1 h. The resulting slurry was filtered onto a 24″Nutsche filter and rinsed [WITH-8°C] to-10°C CH3CN (24 kg) sending the filtrate and rinse to the 1200 L receiver. The filter cake was dried with [50°C] to [55°C] nitrogen to afford another 2.98 kg [ET3NHCL] (9percent yield). The filtrate was transferred to the 1200 L reactor with a CH3CN (10 kg) rinse, and distilled under vacuum to an oil of the title compound of 97.99percent GC purity. The yield was quantitative. M. Pt. [134-136°C.] [APOS;H] NMR (400 MHz, CDC13) : [6] 7.55-7. 40 (6H, br s), 7.25 (6H, t, J = 7. 9 Hz), 7.14 (3H, t, [J =] 7.1 Hz), 3.21-3. 13 (2H, [M),] 3. [10-2. 90 (1H,] br s), 2.94 (2H, t, J = 13.0 Hz), 1.60 [(1H,] br s), 1.48 (1H, br s), 1.15 (1H, br s), 0.94 (3H, d, J = 6.1 Hz), 0.00 (TMS, reference). [13C] NMR (100 MHz, CDC13) : [6] 129.41 (d), 127.46 (d), 125.96 (d), 125.83 (s), 56.12 (t), 51.23 (d), 48.73 (t), 46.45 (t), 20.05 (q), 0.00 (TMS, reference). IR (diffuse reflectance) 2964,2835, 2483 (w), 2350 (w), 2339 (w), 1956 (w), 1490,1025, 909,742 (s), 717,710 (s), 703 (s), 697 (s), 629, [CM-1.] HRMS [(EI)] calcd for [C24H26N2] 342.2096, found [342. 2101.] [a] [25D=-12° (C 1. 00, CH2CL2).] Anal. Calcd for [C24H26N2] : C, 84.17 ; H, 7.65 ; N, 8.18. Found: C, 84.12 ; H, 7.64 ; N, 7.94.

75336-86-6 (R)-2-Methylpiperazine 7330434, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; BIOVITRUM AB; WO2004/829; (2003); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

192130-34-0, tert-Butyl 4-(2-aminoethyl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step 3: fert-Butyl 4-(2-(nonylamino)ethyl)piperazine-l -carboxylate Chemical Formula: C20H41N3O2 Molecular Weight: 355.57 [00633] To a solution of 1 -bromononane (1.81 g, 8.72 mmol) in MeCN (44 mL) was added 4-(2-aminoethyl)-l-boc-piperazine (2.0 g, 8.72 mmol), K2C03 (2.4 g, 17.4 mmol), and KI (145 mg, 0.872 mmol). The reaction was allowed to stir at 65 °C for 16 hours. The reaction mixture was cooled to room temperature, filtered, and the solids were washed with hexanes. The filtrate was extracted with hexanes, and the combined extracts were concentrated in vacuo. Purification by ISCO silica flash chromatography (0-20percent MeOH/DCM) provided fert-butyl 4- (2-(nonylamino)ethyl)piperazine-l-carboxylate (775 mg, 25percent). UPLC/ELSD: RT = 0.47 min. MS (ES): m/z (MH+) 356.41 for C20H41N3O2 (1738) XH-NMR (300 MHz, CDC13) delta: ppm 3.44 (br. m, 4H); 2.74 (t, 2H); 2.63 (t, 2H); 2.53 (t, 2H); 2.41 (br. m, 4H); 1.48 (br. m, 9H); 1.30 (br. m, 14H); 0.90 (t, 3H)., 192130-34-0

As the paragraph descriping shows that 192130-34-0 is playing an increasingly important role.

Reference：
Patent; MODERNATX, INC.; BENENATO, Kerry E.; BUTCHER, William; (437 pag.)WO2017/112865; (2017); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

1001180-21-7, (R)-tert-Butyl 4-(5-methyl-7-oxo-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazine-1-carboxylate is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Example 40; 2-(4-chlorophenyl)-l-(‘4-((5R)-7-hydroxy-5,7-diniethyl-6,7-dihvdro-5H-cvclopenta[dlpyrimidin-4- vDpiperazin- 1 -ylV S-fisopropylamino’propan- 1 -one; Step 1 :; A solution of (R)-tert-butyl 4-(5-methyl-7-oxo-6,7-dihydro-5H- cyclopenta[d]pyrimidin-4-yl)piperazine-l-carboxylate (40 nig, 0.120 mmol) in THF (4 niL) was added to a 1.5M solution of methyllithium in diethyl ether (0.088 mL, 0.132 mmol) at -780C. The resulting mixture was stirred at -78C for 1 hour and quenched by saturated aqueous NH4Cl. The aqueous layer was extracted with EtOAc (2 X). The organic layer was dried (MgSO^ and concentrated. The residue was purified by a silica catridge (5.0 g) eluted by EtOAc to give tert-butyl 4-((5R)-7-hydroxy-5,7-dimethyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-4-yl)piperazine- 1-carboxylate as an off-white solid (29 mg, 69%). LCMS (APCI+) [M-Boc+H]+ 349.1; Rt: 2.49 min.

1001180-21-7, The synthetic route of 1001180-21-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; ARRAY BIOPHARMA INC.; GENENTECH, INC.; MITCHELL, Ian, S.; BLAKE, James, F.; XU, Rui; KALLAN, Nicholas, C.; XIAO, Dengming; SPENCER, Keith, Lee; BENCSIK, Josef, R.; LIANG, Jun; SAFINA, Brian; ZHANG, Birong; CHABOT, Christine; DO, Steven; WO2008/6040; (2008); A1;,
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.16154-72-6,3-Chloro-4-(4-methylpiperazin-1-yl)benzenamine,as a common compound, the synthetic route is as follows.

[00499] A mixture of 6-chloro-4-(2,4-dichlorophenylthio)-1H-indole-2-carboxylic acid (100 mg, 0.27 mmol), 3-chloro-4-(4-methylpiperazin-1-yl)benzenamine (122 mg, 0.54 mmol), HATU (156 mg, 0.41 mmol), Et3N (136 mg, 1.35 mmol) in DMF (5 mL) was stirred for 16 h at rt. The reaction was quenched with water (10 mL) and extracted with ethyl acetate (20 mL). The organic phase was washed water (10 mL x 2), and brine (10 mL), dried (Na2S04), filtered and concentrated in vacuo and the residue was purified by prep-HPLC (0.01%TFA) to afford 6-chloro-N-(3-chloro- 4-(4-methylpiperazin-1-yl)phenyl)-4-(2,4-dichlorophenylthio)-1H-indole-2-carboxamid (TFA salt) I-lll (56.0 mg, 0.08 mmol, 30%) as a white solid. ESI-MS (EI+ m/z): 581.0 [M+H]+. 1H MR (500 MHz, DMSO) delta 12.32 (d, J= 1.5 Hz, 1H), 10.41 (s, 1H), 9.86 (s, 1H), 7.96 (d, J= 2.5 Hz, 1H), 7.77 (d, J= 2.5 Hz, 1H), 7.71 (dd, J= 8.5 Hz, J= 2 Hz, 1H), 7.63 (s, 1H), 7.31-7.25 (m, 3H), 6.72 (d, J= 8.5 Hz, 1H), 3.52 (s, 2H), 3.49 (s, 2H), 3.24 (s, 2H), 3.00 (s, 2H), 2.88 (s, 3H)., 16154-72-6

The synthetic route of 16154-72-6 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; NAVITOR PHARMACEUTICALS, INC.; MAHONEY, Sarah; MOLZ, Lisa; NARAYAN, Sridhar; SAIAH, Eddine; (516 pag.)WO2018/191146; (2018); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics