Tag: M.W:200-300

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows., 7411-23-6

chloroacetone (0.7 mL, 8.8 mmol) was slowly added to a solution of 3,5-dibromo-1H-1,2,4-triazole (1000 mg, 4.4 mmol), triethylamine (1.84 mL, 13 mmol) and DMF (20 mL) at RT and the reaction mixture was stirred at 65 oC for 3 h and RT for 2 days. The reaction mixture was quenched with NH4Cl (sat. aq.) and extracted with DCM. The combined organic fractions were dried with a phase separator and reduced in vacuo. The residue was dissolved in DCM and reduced onto silica and purified by silica column chromatography eluting with 10-90% EtOAc in Pet. Ether to afford 1-(3,5-dibromo-1,2,4-triazol-1-yl)propan-2-one (1102 mg, 3.9 mmol, 88% yield) as a white solid. UPLC-MS (ES+, Method A): 1.19 min, m/z 283.9 [M+H]+

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; REDX PHARMA PLC; JONES, Clifford, D.; BUNYARD, Peter; PITT, Gary; BYRNE, Liam; PESNOT, Thomas; GUISOT, Nicolas, E.S.; (318 pag.)WO2019/145729; (2019); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

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. 1533519-84-4 name is 4-(4-Cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione, 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. 1533519-84-4

To a 250 mL reaction flask was added 4-(4-cyclopropylnaphthalen-1-yl)-4Eta-1,2,4-triazole-3-thiol (Compound A, 58, 0.01811101), potassium carbonate (3.748, 0.02711101, 1.569), 01 ^ (5011 ^). Ethyl bromoacetate was added dropwise with stirring (3.3 g, 0.022 mol 1,1.2 eq). After completion of the reaction, the reaction was stirred at room temperature for 1.5 h. Sampling After testing the raw material, the reaction is complete, Should be added to the liquid ice water 1OOmL, a white solid precipitation. Stir for 30min, suction filter, washed. After the cake was dried, the residue was washed with ethyl acetate Recrystallization gave

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

Reference:
Patent; Zhejiang Jingxin Pharmaceutical Co., Ltd.; Shanghai Jingxin Bio-pharmaceutical Co., Ltd.; Dai Xiangqian; Huang Yue; (17 pag.)CN107098866; (2017); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

A common compound: 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, belongs to Triazoles compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 7411-23-6

In a 100 mL round bottomed flask, 3,5-dibromo-1H-1,2,4-triazole (lnt-1, 2.50 g, 11 mmol) was dissolved in DMF (32 mL) and the solution was cooled to 0-5 C (ice bath). Sodium hydride (55% dispersion in mineral oil, 577 mg, 13.2 mmol) was added in portions and the resulting mixture was stirred for 5 min at 0-5 C and for 15 min at room temperature. After that, ethyl methanesulfonate (2.74 g, 2.27 mL, 22 mmol) was added dropwise at room temperature. The resulting mixture was stirred for 1.5 h at 100 C, and 16 h at room temperature. After that, it was concentrated in vacuo, the residue was diluted with ethyl acetate (100 mL) and water (100 mL), the aqueous phase was extracted with ethyl acetate (3 x 100 mL). The combined organic layers were dried (sodium sulfate) and concentrated in vacuo, the residue was purified by column chromatography (silica gel, 70 g, eluting with ethyl acetate / n-heptane, gradient 0: 100 to 22:78 v/v) to yield the title compound as white solid (1.98 g, 70%). HPLC (method LCMS_fastgradient) tR = 0.88 min. 1H NMR (CDCl3, 300 MHz): delta 1.49 (t, J = 7.2 Hz, 3 H), 4.21 (q, J= 7.2 Hz, 2 H). MS (ES+) m/z 253.9, 255.9, 258.0 [M+H, 2 Br isotopes] .

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, 7411-23-6, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; BARTELS, Bjoern; BERCHTOLD, Stefan; GALLEY, Guido; GOERGLER, Annick; JAKOB-ROETNE, Roland; KRUMMENACHER, Daniela; LIMBERG, Anja; NEIDHART, Werner; RATNI, Hasane; REUTLINGER, Michael; RODRIGUEZ SARMIENTO, Rosa Maria; SCHNIDER, Christian; (309 pag.)WO2018/87018; (2018); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

1533519-84-4, 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. 1533519-84-4, name is 4-(4-Cyclopropylnaphthalen-1-yl)-1H-1,2,4-triazole-5(4H)-thione, A new synthetic method of this compound is introduced below.

The reaction flask was added to 250mL of 4- (4-cyclopropyl-naphthalen-1-yl) -4H-1,2,4- triazole-3-thiol (compound A, 5g,0.018mol), potassium carbonate (3.74g, 0.027mol, 1.5eq), DMF (50ml). Stirring solution of ethyl bromoacetate (3.3g,0.022mol, 1.2eq). Dropping was completed, the reaction was stirred room temperature for 1.5h. Sample testing of raw materials after completion of the reaction, to the reaction mixture was stirred atWas added dropwise in ice water 100ml, white solid was precipitated. Stirring 30min, filtration, washing with water. After drying the filter cake with acetic acidRecrystallized from ethyl to give a white solid 4g, i.e. intermediates B.

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; Zhejiang Jingxin Pharmaceutical Co., Ltd.; Huang, yue; Xu, hui; Zhangyu, bin; Zheng, fei; (19 pag.)CN105399694; (2016); A;,
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. 7411-23-6, name is 3,5-Dibromo-1H-1,2,4-triazole, A new synthetic method of this compound is introduced below., 7411-23-6

A solution of 1.4 g (36 mmol) of sodium hydroxide in13 mL of water was added to a solution of 8.0 g (36 mmol) of 3,5-dibromo-1H-1,2,4-triazole (1) in100 mL of acetone. The two-phase system thus formed was stirred at 20 C until it became homogeneous, and 4.6 g (36 mmol) of dimethyl sulfate was added dropwise at such a rate that the temperature of the mixture did not exceed 40 C. The mixture was then refluxed for 2 h. The reaction was assumed to be complete when the mixture became weakly acidic and sodium methyl sulfate precipitated. The mixture was filtered,and the solvent was distilled off from the filtrate under reduced pressure. The residue was washed with water, and the precipitate was filtered off and recrystallized from hexane. Yield 7.8 g (88 %), mp 64-65 C [22]. IR spectrum, nu, cm-1: 2951, 1717, 1699, 1464, 1418,1391, 1354, 1275, 1250, 1115, 1016, 989, 712, 700. 1H NMR spectrum, delta, ppm: 3.87 s (3H, CH3). 13C NMR spectrum, deltaC, ppm: 37.4 (CH3), 131.3 (C3),139.1 (C5). Mass spectrum, m/z (Irel, %): 243 (51.1) [M]+, 241 (100) [M]+, 239 (48.9) [M]+, 229 (21.3), 227 (48.3), 225 (24.2), 218 (1.2), 200 (6.1), 198 (12.3), 196 (5.1), 162 (14.5), 160 (13.1), 136 (33.4), 134 (34.9), 122 (30.6), 120 (31.3), 119 (6.3), 117 (7.4), 108 (14.6), 107 (7.7), 106 (16.2), 105 (8.9), 93 (15.9), 91 (18.9), 81 (40.9), 79 (32.5), 52 (12.7), 43 (33.8), 41 (12.2), 40 (13.3), 39 (9.1), 38 (18.5), 29 (53.2), 28 (10.7), 27(16.3), 26 (8.2), 15 (60.3), 12 (7.4).

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; Tolstyakov; Russian Journal of Organic Chemistry; vol. 54; 10; (2018); p. 1537 – 1547; Zh. Org. Khim.; vol. 54; 10; (2018); p. 1525 – 1534,10;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics