Tag: M.W:100-200

115761-79-0, 1-(2,4-Difluorophenyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 30; 7-(2-(4-(2,4-Difluorophenyl)piperazin-1-yl)ethyl)-2-(furan-2-yl)-7H-pyrrolo[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5-amine, Method E; A. 4-Chloro-7-(2-(4-(2,4-difluorophenyl)piperazin-1-yl)ethyl)-7H-pyrrolo[2,3-d]pyrimidin-2-amine; To a solution of the title A compound in Example 29, 7-(2-bromoethyl)-4-chloro-7H-pyrrolo[2,3-d]pyrimidin-2-amine (225 mg, 0.817 mmol) and 1-(2,4-difluorophenyl)piperazine (193 mg, 0.976 mmol) in 1 mL of dry acetone is added potassium carbonate (322 mg, 2.44 mmol). The mixture is heated at 50 C. for 24 h, cooled to RT, concentrated in vacuo, and the residue taken up in water. The aqueous mixture is repeatedly extracted with EtOAc, and the combined organic extracts are dried (Na2SO4), filtered and evaporated to dryness. The residue is purified by column chromatography on silica gel, eluting with 2% MeOH in DCM to afford 4-chloro-7-(2-(4-(2,4-difluorophenyl)piperazin-1-yl)ethyl)-7H-pyrrolo[2,3-d]pyrimidin-2-amine as a yellow solid: 1H NMR (CDCl3) delta 2.68 (m, 4H), 2.77 (t, 2H, J=8.0 Hz), 3.01 (m, 4H), 4.19 (t, 2H, J=8.0 Hz), 4.88 (br s, 2H), 6.36 (d, 1H, J=4.0 Hz), 6.77-6.87 (m, 3H), 6.96 (d, 1H, J=4.0 Hz).

115761-79-0, 115761-79-0 1-(2,4-Difluorophenyl)piperazine 2734637, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; Moorman, Allan R.; US2008/242672; (2008); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

75336-86-6,75336-86-6, (R)-2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Part A Synthesis of (R)-1-(3-Chloro-pyridin-2-yl)-3-methyl-piperazine: Dissolve 2,3-dichloropyridine (8.5 g, 0.057 moles) and (R)-(-)-2-methylpiperazine (5.75 g, 0.057 moles) in N,N-dimethylacetamide (125.0 mL) under nitrogen atmosphere. Add anhydrous powdered K2CO3 (23.75 g, 0.172 moles) to this mixture and stir at 135-140° C. for 48 h. New spot noticed in TLC (5percent MeOH / CHCl3 / 1percent NEt3) along with absence of starting materials. Cool the reaction mixture to room temperature, dilute with water (400 mL), extract with EtOAc (3*200 mL) and wash the combined organic extract with brine (2*150 mL). Dry over MgSO4, concentrate under vacuum to afford crude product (20.0 g) as orange yellow liquid. Distil the crude under high vacuum to afford pyridylpiperazine derivative as yellow viscous oil (10 g, bp 112-115° C. /0.1 torr). NMR (CDCl3): delta.. 1.1-1.12 (d, 3H, J=1.6 Hz), 2.50-2.53 (t, 1H), 2.83-2.87 (m, 1H), 3.06-3.08 (m, 3H), 3.67-3.75 (m, 2H), 6.80-6.82(dd, 1H), 7.56-7.58 (dd, 1H), 8.17-8.18 (dd, 1H).

As the paragraph descriping shows that 75336-86-6 is playing an increasingly important role.

Reference：
Patent; Bakthavatchalam, Rajagopal; Hutchison, Alan; DeSimone, Robert W.; Hodgetts, Kevin J.; Krause, James E.; White, Geoffrey G.; US2002/132853; (2002); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

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

103-76-4, N-(2-Hydroxyethyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

20 mmol of 4,6-dichloro-2-methylpyrimidine, 40mmol K3PO4 was dissolved in 100mL N,N-dimethylacetamide, stirring,0.3 mmol of 1-butyl-3-methylimidazolium glycinate and 22 mmol of N-hydroxyethylpiperazine were added in this order, and the mixture was reacted at 80 C for 2 h, and then cooled to room temperature. Add 22 mmol of 2-amino-N-(2-chloro-6-methylphenyl)-5-thiazolecarboxamide, The reaction was continued at 80 C for 3 h. After the reaction was completed, it was cooled to room temperature and poured into ice water. It was extracted with ethyl acetate three times (3×50 mL), and the ethyl acetate phase was combined. The organic layer was washed with anhydrous Na2SO4 to give a crude product. The crude product was added to 100 mL of an 80% aqueous ethanol solution, and 2 g of activated carbon was added thereto with stirring. After refluxing for 30 min, it was filtered while hot, and the filtrate was recrystallized overnight and filtered. The filter cake was washed with ice-cold 80% aqueous ethanol and dried. That is, 8.72 g of a white solid was obtained, the yield was 89.31%, and the purity was 99.94%., 103-76-4

The synthetic route of 103-76-4 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Shandong Luoxin Pharmaceutical Group Co., Ltd.; Shandong Luoxin Pharmaceutical Group Hengxin Pharmaceutical Co., Ltd.; Shandong Yuxin Pharmaceutical Co., Ltd.; Li Mingjie; Li Chenglong; Li Cheng; (12 pag.)CN109678853; (2019); A;,
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

Palladium (II) acetate (941 mg, 4.2 mmol) and rac-2,2′-bis(diphenylphosphino)-1,1′-binapthyl (3.93 g, 6 mmol) were heated to 50°C in dioxane (200 ml) for 30 minutes. Cesium carbonate (20.48 g, 63 mmol), 4-bromo-2-nitroanisole (9.75 g, 42 mmol) and cis-2,6-dimethylpiperazine (14.39 g, 126 mmol) were added and the mixture heated at reflux for 18 hours. The solids were filtered through celite and washed with ethyl acetate. The residue was concentrated and dissolved in ethyl acetate and extracted with 2N hydrochloric acid (x5). The combined extracts were washed in ethyl acetate (x3), basified with 0.880 ammonia and extracted with dichloromethane (x5). The combined organic extracts were concentrated, redissolved in ethyl acetate and washed with water (x3), saturated brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified by column chromatography (Biotage Horizon, dichloromethane to 1:9 2M ammonia in methanol:dichloromethane) to afford the titleproduct (D3). MS (ES+) m/e 266 [M+H]+., 21655-48-1

The synthetic route of 21655-48-1 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; GLAXO GROUP LIMITED; WO2006/10629; (2006); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

4318-42-7, 1-Isopropylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Oxalyl chloride (47.7 kg, 375.8 mol) was added to a solution of oxazole-5-carboxylic acid (32.88 kg, 290.8 mol) in isopropyl acetate (144 kg) maintaining the temperature at 52-58 °C. The temperature was increased to 58.5 °C, stirred for 5 h and then cooled to 20 °C. The reactionmixture was added to a solution of 1-(isopropyl)piperazine (41 kg, 319.8 mol) and potassium carbonate (118.4kg) in isopropyl acetate (348 kg) and water (103 kg) maintaining the temperature below 25 °C. The reaction was stirred for 15 mins, the temperature was increased to 33 °C and the organic phase washed with water (191 kg), concentrated under reduced pressure to 95 L and cooled to 20 °C. n-Heptane (157 kg) was added and the crystallisation stirred for 2 h, and theproduct filtered off, washed with n-heptane (157 kg) and dried under vacuum 40 °C to give the title compound (57.14 kg, 88.0percent).1H NMR (400 MHz, CDCI3-d) ppm 7.94 (5, 1 H), 7.56 (5, 1 H), 3.91-3.73 (m, 4 H), 2.75 (spt., J=6.5 Hz, 1 H), 2.63-2.52 (m, 4 H) and 1.06 (d, J=6.6 Hz, 6 H)., 4318-42-7

The synthetic route of 4318-42-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY DEVELOPMENT LIMITED; BREAM, Robert Nicholas; HAYLER, John David; IRONMONGER, Alan Geoffrey; SZETO, Peter; WEBB, Michael Robert; WHEELHOUSE, Katherine Marie Penelope; WILLACY, Robert David; (50 pag.)WO2016/193255; (2016); 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.21655-48-1,cis-2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

In a sealed tube, 7-fluoro-2-(2-methylimidazo [1 ,2-b]pyridazin-6-yl)-4H-pyrido [1,2- a]pyrimidin-4-one (Intermediate 1; 50 mg, 0.169 mmol), and cis-2,6-dimethylpiperazine (77mg, 0.677 mmol, 4.0 eq.) were stirred in DMSO (2 mL) at 110C overnight. The solvent was removed under high vacuum. The residue was taken up in CH2C12 and washed with an aqueous saturated solution of NaHCO3. The organic layer was separated and dried over Na2504 and concentrated in vacuo. The crude was purified by column chromatography (5i02, CH2C12/MeOH=95/5 to 90/10) to afford the title product (41 mg, 62%) as a light yellow solid.MS m/z 390.3 [M+H?i., 21655-48-1

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

Reference：
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; ALSENZ, Jochem; GRASSMANN, Olaf; KUEHL, Peter; METZGER, Friedrich; MCCARTHY, Kathleen Dorothy; MORAWSKI VIANNA, Eduardo Paulo; WOODHOUSE, Marvin Lloyd; (130 pag.)WO2017/80967; (2017); 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.21655-48-1,cis-2,6-Dimethylpiperazine,as a common compound, the synthetic route is as follows.

[14031 Step 1: Synthesis of (E?)-methyl3-(4-(((3R.55?)-3 .5-dimethylpiperazin- 1 -yl?)methyl?)phenyl?)acrylate [14041 (2S ,6R)-2,6-dimethylpiperazine (0.500 g, 4.379 mmol), (E)-methyl3-(4-(bromomethyl)phenyl)acrylate (formula 8-4, 1.173 g, 4.598 mmol) and Cs2CO3 (2.140 g, 6.568 mmol) were dissolved in acetonitrile (10 mL) at room temperature, and the reaction solution was stuffed at the same temperature for 5 hours. Then, the reaction mixture was filtered through a glass filter to remove solids, and the filtrate was con-centrated under reduced pressure. The concentrate was purified by column chromatography (silicon dioxide, 12 g cartridge; methanol/methylene chloride = from 0 percent to 15 percent) and concentrated to afford the desired compound (1.090 g, 86.3 percent) as an orange solid., 21655-48-1

21655-48-1 cis-2,6-Dimethylpiperazine 6950261, apiperazines compound, is more and more widely used in various fields.

Reference：
Patent; CHONG KUN DANG PHARMACEUTICAL CORP.; SONG, Hyeseung; LEE, Changgon; KWAK, Dalyong; LEE, Jaeyoung; BAE, Suyeal; KIM, Yuntae; BAE, Daekwon; HA, Nina; BAE, Miseon; KIM, Jihyun; WO2015/137750; (2015); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

13754-38-6, 1-Benzoylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

General procedure: A solution of 2-chloroalkyl/aryl substitutedwith or without N-substitution as well as with or without 5 and/or 6-substituted benzimidazole derivative (1.75g,0.01051mol) and 1-[(4-phenyl)carbonyl]piperazine (3g,0.0105mol) in N, N dimethylformamide was taken in a RBF.K2CO3(2gm,) was added to the reaction mixture. The reaction mixture was stirred for 8h at 80C on a magnetic stirrer (heat + stirring). The progress of the reaction was monitored by thin layer chromatography (TLC).Upon completion of the reaction, water was added to the reaction mixture and the product extracted by shaking the reaction mixture with dichloromethane in a separating funnel.The dichloromethane layer was washed successively with water and brine, dried over anhydrous sodium sulfate. Evaporation of the solvent gave theproduct. 11a-l Recrystallized with various solvent like chloroform, ethanol, methanol., 13754-38-6

As the paragraph descriping shows that 13754-38-6 is playing an increasingly important role.

Reference：
Article; Kankate, Rani S.; Gide, Parag S.; Belsare, Deepak P.; Oriental Journal of Chemistry; vol. 30; 4; (2014); p. 1855 – 1863;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics

59702-07-7, 1-Methylpiperazin-2-one is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

59702-07-7, A mixture N [5-chloro-7- (3-methoxyprop-1-yn-1-yl)-1, 3-benzodioxol-4-yl]-7- (3- chloropropoxy) -5-isopropoxyquinazolin-4-amine (0.320 g, as a 1: 1.3 wt.: wt. mixture with triphenylphosphine) and 1-methylpiperazin-2-one (0.280 g) was dissolved in 2- methoxyethanol (7 ml), then sodium iodide (0.040 g) was added and the reaction mixture was then heated at 110°C with stirring for 24 hours. The reaction mixture was then cooled to room temperature, diluted with dichloromethane (70 ml) and washed with water: brine (1: 1) then water then brine and dried over magnesium sulfate before filtration and evaporation of solvents under reduced pressure. The residues so resulting were then purified by column chromatography on silica using increasingly polar mixtures of methanol in dichloromethane as eluent. There was thus obtained 4- (3- {4- [5-chloro-7- (3-methoxy-prop-1-ynyl)- benzo [1, 3] dioxol-4-ylamino]-5-isopropoxy-quinazolin-7-yloxy}-propoxy)-1-methyl- piperazin-2-one (0.086 g) as a white foam; NMR Spectrum: (CDC13) 1.53 (d, 6H), 2.02 (quin, 2H), 2.61 (t, 2H), 2.72 (t, 2H), 2.96 (s, 3H), 3.18 (s, 2H), 3.33 (t, 2H), 3.45 (s, 3H), 4.15 (t, 2H), 4.35 (s, 2H), 4.83 (sept, 1H), 6.10 (s, 2H), 6.49 (d, 1H), 6.82 (d, 1H), 7.05 (s, 1H), 8.51 (s, 1H), 9.41 (s, 1H); Mass Spectrum: M+H+ 596/598.

As the paragraph descriping shows that 59702-07-7 is playing an increasingly important role.

Reference：
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2004/4732; (2004); A1;,
Piperazine – Wikipedia
Piperazines – an overview | ScienceDirect Topics