Category: 1455-77-2

Application of 1455-77-2, 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. 1455-77-2 name is 3,5-Diamino-1,2,4-triazole, 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.

1H-1,2,4-Triazole-3,5-diamine (12.4 g, 0.125 mol) was dissolved in AcOH (50 ml), and diethyl 2-(ethoxymethylene)malonate (32.5 g, 0.15 mol) was added. The solution was refluxed overnight, then cooled, filtered, and dried to give Key Intermediate VI (22 g, 79percent) as a white solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diamino-1,2,4-triazole, and friends who are interested can also refer to it.

Reference:
Patent; European Molecular Biology Laboratory; F. Hoffmann-La Roche AG; WOLKERSTORFER, Andrea; SZOLAR, Oliver; HANDLER, Norbert; CUSACK, Stephen; SAUVAITRE, Thibault; SIMON, Celine; MORICE, Christophe; GIETHLEN, Bruno; LANGER, Thierry; SMITH, Mark; SO, Sung-Sau; CLASSEN-HOUBEN, Dirk; BUSCHMANN, Helmut; US2013/317022; (2013); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

1455-77-2, name is 3,5-Diamino-1,2,4-triazole, belongs to Triazoles compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. HPLC of Formula: C2H5N5

2-Hydroxybenzaldehyde (0.02 mol L1, 2 mL) in ethanol (10 mL)was added to a magnetically stirred solution of 3,5-diamino-1,2,4-triazole (0.01 mol L1, 0.99 mg) in ethanol (20 mL). The mixture was refluxed for 2 h. The reaction was monitored through TLC.During refluxing yellow precipitates started forming. It was refluxed for another half an hour. It was then cooled to room temperature, filtered, washed with cold ethanol (2 10 mL) thenwith ether (2 5 mL), dried and recrystallized in a mixture of hot ethanol and ether (2:1).2.3. 2-{(E)-[(3-{[(Z)-(2-hydroxyphenyl)methylidene]amino}-1H-1,2,4-triazol-5-yl)imino]methyl}phenol (L)Yield: (1.63 g, 75percent); mp: 244 ¡ãC; color (yellow): IR (cm-1): 3429(OH), 3195 (N-H), 1634 (HC=N), 1604 (C=N) and 1023 (N-N); 1HNMR (ppm DMSO?d6): d 12.81 (s, 1H, NH), 12.14 (s, 1H, OH), 9.16 (s,2H, C7-H, C7,-H), 6.97-7.69 (m, Ar-H); 13C NMR (DMSO?d6):d 157.19 (C8,C8,), 160.67 (C7,C7,), 168.54 (C1, C1,), 117.05-133.93(Ar-C); Mass Spectrum EIMS m/z (percent): 307.31: [M], 308.0(10),277.1(17), 204.1(13), 185.1(100), 171.1(6), 157.0(4). Anal. Calc. for C16H13N5O2 (307.31): C, 62.53 (62.45); H, 4.26 (4.20); N, 22.79(22.72).

The synthetic route of 1455-77-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Sumrra, Sajjad Hussain; Kausar, Samia; Raza, Muhammad Asam; Zubair, Muhammad; Zafar, Muhammad Nadeem; Nadeem, Muhammad Arif; Mughal, Ehsan Ullah; Chohan, Zahid Hussain; Mushtaq, Fazila; Rashid, Umer; Journal of Molecular Structure; vol. 1168; (2018); p. 202 – 211;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Related Products of 1455-77-2, A common heterocyclic compound, 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, molecular formula is C2H5N5, 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.

General procedure: A suspension of 3,5-diamino-1,2,4-triazole (0.1 g, 1 mmol) in absolute EtOH (10 mL) was added to a stirring solution of azo-coupled precursors, Ia-IVa, (2 mmol) in absolute EtOH (50 mL) during a period of 10 min at 60-70 ¡ãC. The mixture was heated in water bath for 15 h at 80 ¡ãC with stirring. The mixture was filtered whilst hot and the obtained solid was washed with hot ethanol (three time) and then with diethylether. The resulted product was dried in air.

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; Khanmohammadi, Hamid; Erfantalab, Malihe; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 86; (2012); p. 39 – 43;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, belongs to Triazoles 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 1455-77-2, Computed Properties of C2H5N5

General procedure: A total of 2.47 g (0.01 mol) 2,4,6-trinitrochlorobenzene (picrylchloride) was dissolved in 50 mL MeOH by heating in a two-necked flask. Then, the solution was heated up to its boiling point under reflux. There was 0.01 mol solution of amino-heterocyclic compound in 20 mL hot MeOH added to it. It was heated under reflux for 4 h evaporating to the half. The yellow productwas filtered off and dried in air.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diamino-1,2,4-triazole, and friends who are interested can also refer to it.

Reference:
Article; Yigiter, Aynur Ozler; Atakol, Melike Kundurac?; Levent Aksu; Atakol, Orhan; Journal of Thermal Analysis and Calorimetry; vol. 127; 3; (2017); p. 2199 – 2213;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, belongs to Triazoles 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 1455-77-2, name: 3,5-Diamino-1,2,4-triazole

Example 11AEthyl 2-amino-7-(4-cyanophenyl)-5-methyl-4,7-dihydro[1,2,4]triazolo[1,5-a]pyrimidine-6-carboxylateUnder an atmosphere of argon, ethyl 2-(4-cyanobenzylidene)-3-oxobutanoate (12.2 g, 50.1 mmol; preparation see WO 2004/020410-A2, Example 32A) and 1H-1,2,4-triazole-3,5-diamine (6.0 g, 60.5 mmol, 1.2 eq.) were dissolved in DMF (150 ml).Solid sodium bicarbonate (30.7 g, 365.6 mmol, 6 eq.) was added, and the mixture was stirred at 63¡ã C. for 12 h.The mixture was then filtered and the DMF was distilled off from the filtrate under reduced pressure.The residue was suspended in ethanol and stirred, and the product was then filtered off and dried under high vacuum.This gave 12.45 g (76percent of theory) of the title compound.LC-MS (Method 4): Rt=2.29 min; MS (ESIpos): m/z (percent)=325.3 (100) [M+H]+; MS (ESIneg): m/z (percent)=323.3 (100) [M+H]-.1H-NMR (400 MHz, DMSO-d6): delta=1.00 (t, 3H), 2.40 (s, 3H), 3.95 (m, 2H), 5.25 (s, 2H), 6.05 (s, 1H), 7.35 (m, 2H), 7.75 (m, 2H), 10.6 (s, 1H).

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:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; US2012/4203; (2012); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – 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. 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, A new synthetic method of this compound is introduced below., Recommanded Product: 3,5-Diamino-1,2,4-triazole

2-acetylthiophene (8.20 g) and N,N-dimethylformamide diethyl acetal (13.6 mL) were heated to reflux at 130¡ãC in xylene (13 mL) for two days. The reaction liquid was concentrated under reduced pressure, and after subjected to azeotropic distillation with toluene, crystallized with a mixed solvent of toluene-hexane and 3-dimethylamino-1-thiophen-2-ylpropenone (11.52g, yield 98percent) was obtained. The obtained 3-dimethylamino-1-thiophen-2-ylpropenone (10.78 g) was dissolve in toluene (160 mL) and stirred at 100¡ãC with 3,5-diamino-1,2,4-triazole (14.15 g) added. After 10-camphor sulfonic acid (13.82 g) was added, it was heated to reflux for 1.5 hours. After having cooled to room temperature, the supernatant was removed (decantation). The residue was suspended and washed with 5percent sodium carbonate/10percent ethanol aqueous solution, 10percent ethanol water, absolute ethanol and methylene chloride in this order and dried under reduced pressure and the title compound was obtained (8.55 g, yield 66percent).

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:
Patent; NIPPON KAYAKU KABUSHIKI KAISHA; EP1674454; (2006); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Reference of 1455-77-2, A common heterocyclic compound, 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, molecular formula is C2H5N5, 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.

A mixture of Zn(NO3)2¡¤6H2O (0.030 g, 0.1 mmol), H3btc (0.024 g, 0.1 mmol), Hdatrz (0.01 g, 0.10 mmol), NaHCO3 (0.025 g, 0.3 mmol) and H2O (10 mL) was placed in a 23 ml Teflon-lined stainless steel reactor under autogenous pressure at 160 ¡ãC for 60 h and then cooled to the room temperature slowly. Colorless prism crystals were obtained in 34percent yield based on Zn(NO3)26H2O. Anal. calcd. for C11H7N5O6Zn2 (436.00): C, 30.28; H, 1.61; N, 16.06percent. Found: C, 30.31; H, 1.58; N, 16.02percent. IR (KBr, cm?1) 3387(s), 3175(m), 1607(s), 1566(s), 1395(s), 1366(m), 1307(w), 1224(m), 1077(s), 853(w), 718(s), 688(m), 647(w).

The synthetic route of 1455-77-2 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Cui, Penglei; Li, Xiaohui; Journal of Molecular Structure; vol. 1081; (2015); p. 182 – 186;,
1,2,3-Triazole – Wikipedia,
Triazoles – 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. 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, A new synthetic method of this compound is introduced below., Safety of 3,5-Diamino-1,2,4-triazole

Added to three neck fever bottle 126mmol stearic acid, 60mmol3,5-diamino -1, 2, 4-three nitrogen […] 21g glycol solvent, under the protection of argon gas, heating 80 ¡ãC after melting, by adding 3mmol potassium hydroxide, wherein stearic acid: 3,5-diamino -1, 2, 4-triazole: potassium hydroxide mole ratio is 2.1: 1 : 0.05, glycol as the above-mentioned reactant of the total weight of the 50percent. Continued heating to 150 ¡ãC, reaction 12h rear, with 1percent sodium carbonate water solution, in order to remove unreacted stearic acid and the solvent is ethylene glycol, drying to obtain yellow solid containing heterocyclic stearic acid amide-based intermediate A.

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:
Patent; China Petroleum & Chemical Corporation; Yu, Jianye; Lu, Minhui; Yuan, Ping; Yuan, Yufeng; (9 pag.)CN105693640; (2016); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 1455-77-2, A common heterocyclic compound, 1455-77-2, name is 3,5-Diamino-1,2,4-triazole, molecular formula is C2H5N5, 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.

Example 312-amino-6- [(4-fluorophenyl)methyl] -5-methyl-4H- [ 1 ,2,4] triazolo [5,1-b] pyrimidin-7- oneEthyl 2-[(4-flourophenyl)methyl]-3-methyl-3-oxo-propanoate (314 mg , 1.32 mmol was added to 3-amino-5-amino-triazole (100 mg, 1.2 mmol) followed by glacial acetic acid (2.0 mL) and the reaction was heated at 120 ¡ãC under microwave irradiation for 15 minutes The solvent was evaporated and then basified with sodium hydrogencarbonate. The formed precipitate was filtered and washed with water, dichloromethane and MeCN to give the title compound (160 mg 49percent)1H NMR (400 MHz, DMSO-d6) 2.27 (3H, s), 3.77 (2H, s), 5.95 (2H, s), 7.06 (2H, d), 7.23- 7.25 (2H, m). m/z (ES) (M+H)+ 274.

The synthetic route of 1455-77-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; BENGTSSON, Boel, Ase; BLACKABY, Wesley; CUMMING, John; FAULL, Alan, Wellington; LARSSON, Joakim; NASH, Ian, Alun; OLDHAM, Keith; PAPE, Andrew; WO2011/114148; (2011); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 1455-77-2, 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. 1455-77-2 name is 3,5-Diamino-1,2,4-triazole, 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.

To a stirred solution of IH- 1 ,2,4-triazole-3,5-diamine (1.0 g, 10.1 mmol), methyl 3-oxobutanoate (1.17 g, 10.1 mmol), and 2,4-dichlorobenzaldehyde (1.35 g, 10.1 mmol) in THF (30 mL) and heptane (8 mL) was added piperidine (30 mg, 0.3 mmol) and the reaction was heated to 70 ¡ãC for 2 days. The reaction was concentrated to afford crude methyl 2-amino-7-(2,4-dichlororhohenyl)-5-methyl-4,7-dihydro-[1,2,4]- triazolo[1,5-alpha]pyrimidine-6-carboxylate as a light yellow solid. [00202] HPLC Phenomenex LUNA C-18 4.6 x 50 mm, 0 to 100percent B over 4 minutes, 1 minutes hold time, A = 90percent water, 10percent methanol, 0.1percent TFA, B = 10percent water, 90percent methanol, 0.1percent TFA, RT = 3.03 min, 97percent homogeneity index.[00203] To a stirred solution of crude methyl 2-amino-7-(2,4-dichlorophenyl)-5- methyl-4,7-dihydro-[1,2,4]-triazolo[1,5-fl]pyrimidine-6-carboxylate (10.1 mmol) in CH2Cl2 (100 mL) was added DDQ (2.75 g, 12.1 mmol). The reaction was kept at room temperature for 1 h and was quenched by satd aq NaHCO3 solution. The organic layer was washed with satd aq NaHCO3 and brine prior to drying over anhydrousMgSO4. Filtration, concentration under reduced pressure and purification by silica gel chromatography afforded methyl 2-amino-7-(2,4-dichlorophenyl)-5-methyl-[ 1,2,4]- triazolo[1,5-fir]pyrimidine-6-carboxylate (2.0 g, 56percent) as a light yellow solid. [00204] 1H NMR (400 MHz, CDCl3) delta 7.59 (d, J= 1.8 Hz, 1H), 7.43 (dd, J= 1.8, 7.9 Hz, 1H), 7.29 (d, J= 7.9 Hz, 1H), 4.72 (s, 2H), 3.64 (s, 3H), 2.77 (s, 3H). [00205] HPLC Phenomenex LUNA C-18 4.6 x 50 mm, 0 to 100percent B over 4 minutes, 1 minutes hold time, A = 90percent water, 10percent methanol, 0.1percent TFA, B = 10percent water, 90percent methanol, 0.1percent TFA, RT = 2.85 min, 100percent homogeneity index. [00206] LCMS: Anal. Calcd. for C14H11Cl2N5O2 351.03; found: 352.11 (M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3,5-Diamino-1,2,4-triazole, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; WO2006/71752; (2006); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics