Category: 3112-31-0

Reference of 3112-31-0, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 3112-31-0 name is 1H-Pyrazole-3,5-dicarboxylic acid, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

(A mixture of Dy2O3 (0.187g, 0.5mmol), CuSO4·5H2O (0.125g, 0.5mmol), H3PDC (0.174g, 1.0mmol) and H2O (10mL) was stirred in air for 1h, and then was sealed in a Parr Teflon-lined stainless-steel bomb and heated at 160°C for 3 d, cooled down to room temperature (r.t.) at 2°Ch?1 before the furnace was switched off. The resulting purple, columnar crystals of 1 (ca. 0.30mm in length and 0.20nm in diameter) were collected after washing with water (yield: 76percent, based on CuSO4·5H2O). Elem. Anal. Calcd for C10H16CuDy2N4O19S: C 13.10, H 1.79, N 6.11. Found: C 13.13, H 1.82, N 6.09. IR (KBr pellet cm?1): 3445(s), 1621(s), 1598(s), 1509(m), 1393(m), 1328(s), 1276(m), 1138(w), 1063(w), 1014(w), 853(w), 782(w).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1H-Pyrazole-3,5-dicarboxylic acid, and friends who are interested can also refer to it.

Reference:
Article; Wang, Min; He, Liang; Lin, Qipu; Journal of Solid State Chemistry; vol. 265; (2018); p. 29 – 35;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, A new synthetic method of this compound is introduced below., SDS of cas: 3112-31-0

A mixture of 31.7 g (0.203 mol) of diacid 1 and 125 mL of methanol was saturated with gaseous HCl. The mixture was refluxed for 3 h and left overnight at room temperature. The precipitate was filtered off and washed with methanol. Yield 23.5 g (63%), white crystals, mp 142-143C. IR spectrum, nu, cm-1: 3105 br (NH), 1710 s (C=O), 1240 s (C-O-C). 1H NMR spectrum, delta, ppm: 3.82 s (6H, CH3), 6.36 s (1H, 4-H), 14.43 s (1H, NH).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Article; Kharaneko; Russian Journal of Organic Chemistry; vol. 52; 9; (2016); p. 1322 – 1325; Zh. Org. Khim.; vol. 52; 9; (2016); p. 1334 – 1337,4;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 3112-31-0 as follows. Product Details of 3112-31-0

To a 25 mL reactor, 174.0 mg of 3,5-pyrazoledicarboxylic acid monohydrate and 250.0 mg of copper sulfate pentahydrate powder were added, 5 mL of pyridine and 10 mL of water were added, and after stirring for 15 minutes, the reaction kettle was placed in an oven and heated to 180. °C, reaction for 24 hours; After the reaction is completed, the reaction solution is transferred to a flask, and 2 mL of a saturated aqueous solution of sodium sulfide is added to the reaction solution, and after the precipitation is completed, it is filtered:Add 1M hydrochloric acid solution to the filtrate droplet obtained in the second step, adjust the solution pH=3, and filter;The filtrate obtained in the third step was extracted with an organic solvent dichloromethane (3×20 mL), and the organic phase was collected and dried over anhydrous sodium sulfate for 10 h;The organic phase obtained after the fourth step of drying was concentrated and dried to obtain 100 mg of a white powder, which was designated as sample 1.

According to the analysis of related databases, 3112-31-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chinese Academy Of Sciences Fujian Structure Of Matter Institute; Huang Deguang; Xiang Shiqun; Zhang Xiaofeng; (13 pag.)CN109369617; (2019); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Related Products of 3112-31-0,Some common heterocyclic compound, 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, molecular formula is C5H4N2O4, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: The deionized water (3 mL) was slowly dropped over the mixturesolution containing Cu(NO3)23H2O (0.2 mmol, 48 mg) andpyrazine (0.2 mmol, 16 mg) in water and DMF (4 mL, 1:1 v/v) in15 mL of glass vial. Then, the solution of pyrazole-3,5-dicarboxylicacid (0.2 mmol, 35 mg) in deionized water and ethanol (5 mL,1:1 v/v) was carefully layered over the mixture layer. Then, the vialwas sealed and allowed to stand undisturbed at room temperature. The blue crystals of 1 were obtained after 2 days.

The synthetic route of 3112-31-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Klongdee, Fatima; Boonmak, Jaursup; Moubaraki, Boujemaa; Murray, Keith S.; Youngme, Sujittra; Polyhedron; vol. 126; (2017); p. 8 – 16;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

These common heterocyclic compound, 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. HPLC of Formula: C5H4N2O4

Step 1; To a solution of Compound 14 (60 g, 345 mmol) in methanol (600 mL), under flow of nitrogen, thionyl chloride (75 mL, 1034 mmol) was added at 0C. The solution was then heated at reflux for 4 hours. The reaction mixture was concentrated in vacuo to yield crude product 15 (64.3 g). LC/MS (Method A): 0.93 min, [M+H]+ = 185.

The synthetic route of 1H-Pyrazole-3,5-dicarboxylic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Shionogi & Co., Ltd.; EP2426135; (2012); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Application of 3112-31-0, A common heterocyclic compound, 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, molecular formula is C5H4N2O4, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a 25 mL reactor, 174.0 mg of 3,5-pyrazoledicarboxylic acid monohydrate and 250.0 mg of copper sulfate pentahydrate powder were added, 5 mL of 4-methylpyridine and 10 mL of water were added, and after stirring for 15 minutes, the reaction kettle was placed in an oven. Heating to 180 ° C, the reaction is 24 hours;After the reaction is completed, the reaction solution is transferred to a flask, and 2 mL of a saturated aqueous solution of sodium sulfide is added to the reaction solution, and after the precipitation is completed, it is filtered;adding 1M hydrochloric acid solution to the filtrate droplet obtained in the second step, adjusting the solution pH=3, and filtering;The fourth step: extracting the filtrate obtained in the third step (3×20 mL) using an organic solvent dichloromethane, collecting the organic phase, and drying with anhydrous sodium sulfate for 10 h;the organic phase obtained after the fourth step of drying was concentrated and dried to obtain 71.0 mg of a white powder, which was designated as sample 3.

The synthetic route of 3112-31-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Chinese Academy Of Sciences Fujian Structure Of Matter Institute; Huang Deguang; Xiang Shiqun; Zhang Xiaofeng; (13 pag.)CN109369617; (2019); A;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

These common heterocyclic compound, 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Application In Synthesis of 1H-Pyrazole-3,5-dicarboxylic acid

1H-Pyrazole-3,5-dicarboxylic acid (200 mg, 1.281 mmol), methanamine (2M in THF, 0.705 mL, 1.409 mmol) and HATU (536 mg, 1.409 mmol) were combined in DMF (2 mL). DIPEA (0.448 mL, 2.56 mmol) was added and reaction mixture stirred at rt. under N2 for 2 h. The reaction mixture was concentrated to dryness and used crude for the next step. (0432) LCMS (2 min Formic): Rt = 0.37 min, [MH]+ = 183.1.

The synthetic route of 1H-Pyrazole-3,5-dicarboxylic acid has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GLAXOSMITHKLINE INTELLECTUAL PROPERTY (NO.2) LIMITED; ATKINSON, Stephen John; DEMONT, Emmanuel Hubert; HARRISON, Lee Andrew; LIWICKI, Gemma Michele; LUCAS, Simon Christopher Cranko; PRESTON, Alexander G; SEAL, Jonathan, Thomas; WALL, Ian David; WATSON, Robert J; (0 pag.)WO2018/158212; (2018); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 3112-31-0

To prepare the salt, the 3,5-pyrazoledicarboxylic acid monohydrate (0.8705 g, 0.005 mol) was treated with a 10 percent hydrazine hydrate in a 1:1 molar ratio (2.5 mL, 0.005 mol) in 50 mL of distilled water. The resulting solution was heated over a water bath for about 20 min to obtain a clear solution. This solution (pH = 3.5) was cooled to room temperature and was placed in a vacuum desiccator over calcium chloride for crystallization. Needle-shaped colorless crystals of the title salt are separated after a week, and the crystals were washed with ice-cold absolute alcohol and air-dried. The salt was soluble in cold water, insoluble in alcohol, and was stable in air (yield: 85 percent). Elemental analysis: C (percent): 28.50 (Cald. 29.12); H(percent): 5.10 (5.23); N (percent): 27.93 (27.16); and hydrazine (percent):15.10 (Cald. 15.52).

The synthetic route of 3112-31-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Premkumar, Thathan; Srinivasan, Krishnan; Selvakumar, Rajendran; Rath, Nigam P.; Govindarajan, Subbiah; Journal of Thermal Analysis and Calorimetry; vol. 125; 1; (2016);,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3112-31-0, name: 1H-Pyrazole-3,5-dicarboxylic acid

The mixture solution of Cu(NO3)2*3H2O (0.2 mmol, 48 mg), 4,4′-bipyridine (0.2 mmol, 31 mg) and pyrazole-3,5-dicarboxylic acid(0.2 mmol, 35 mg) in the deionized water (7 mL), DMF (2 mL)and ethanol (3 mL) was sealed in a 20 mL glass vial. Then, the mixturewas heated at 120° C for 1 day and then slowly cooled down toroom temperature. The blue crystals of 3 were obtained. Yield:10 mg (16percent) based on copper salt Anal. Calcd for Cu5C50H46N14O24:C, 38.88; H, 3.00; N, 12.69. Found: C, 38.79; H, 2.85; N, 13.00percent. FTIRpeaks (KBr, cm-1): 3368br (m(OH)), 1646s (mas(OCO)), 1599s (m(CN)), 1533w, 1481w, 1407w, 1387m (ms(OCO)), 1288s, 1224m,1065w, 1020w, 817w, 806w, 778 m. UV-vis (diffuse reflectance,cm-1): 14407.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Article; Klongdee, Fatima; Boonmak, Jaursup; Moubaraki, Boujemaa; Murray, Keith S.; Youngme, Sujittra; Polyhedron; vol. 126; (2017); p. 8 – 16;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 3112-31-0, Formula: C5H4N2O4

3,5-Pyrazoledicarboxylic acid monohydrate (8.02 g, 46.1 mmol) was dissolved in the mixture of dry DMF (35 ml), dry DCM (35 ml) and DIPEA (7.9 ml). l-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI, 3.37 g, 17.6 mmol), HOBt (2.28 g, 16.9 mmol), and DIPEA (3 ml, 2.23 g, 17.3 mmol) were added at RT. The solution was mixed for 10 min. Then, 2-[5-(3,4-dichlorophenyl)- furan-2-yl]ethylamine hydrochloride (3.46 g, 1 1.8 mmol) dissolved in the mixture of dry DCM (35 ml) and DIPEA (2.0 ml, 1.48 g, 11.5 mmol) was dropped to the solution at RT. After stirring overnight water was added. The product was extracted into ethyl acetate. The organic phase was washed with water, dried and evaporated. The crude product was purified by flash chromatography using DCM as an eluent. The product was triturated in hot methanol. NMR (400 MHz, DMSO- ): 2.95 (2H, t), 3.56 (2H, m), 6.33 (IH, d), 7.01 (IH, d), about 7.03 (IH, broad s), 7.61 (IH, distorted dd), 7.63 (IH, distorted d), 7.83 (IH, d), about 8.45 (IH, broad s), about 14.05 (IH, broad s).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1H-Pyrazole-3,5-dicarboxylic acid, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ORION CORPORATION; WOHLFAHRT, Gerd; TOeRMAeKANGAS, Olli; SALO, Harri; HOeGLUNG, Lisa; KARJALAINEN, Arja; KNUUTTILA, Pia; HOLM, Patrick; RASKU, Sirpa; VESALAINEN, Anniina; WO2011/51540; (2011); A1;,
Pyrazole – Wikipedia,
Pyrazoles – an overview | ScienceDirect Topics