Category: 31250-99-4

New discoveries in chemical research and development in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. category: Triazoles

EXAMPLE 4 This Example illustrates the preparation of 1-trityl-5-iodo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (9.95 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (3.71 g) in dry tetrahydrofuran (200 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (22.0 ml, 1.6M solution in hexane). The solution was stirred for ten minutes, then treated rapidly with a solution of iodine (10.0 g) in dry tetrahydrofuran (40 ml). After a further one minute, the mixture was quenched at -50 C. with 0.1M sodium thiosulphate (100 ml) and portioned between dichloromethane and water. The organic layer was washed with water, dried over magnesium sulphate, evaporated under reduced pressure and the residue chromatographed on silica, using dichloromethane-ether (25:2) as eluant to give the title compound (11.73 g, m.p. 248-250 C.). NMR (CDCl3): delta7.1-7.3 (15H,m), 8.0(1H,s). 13 C NMR confirmed position of substitution. M/S: M+ 437

I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 1-Trityl-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 31250-99-4, New Advances in Chemical Research in 2021. Chemo-enzymatic cascade processes are invaluable due to their ability to rapidly construct high-value products from available feedstock chemicals in a one-pot relay manner. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

EXAMPLE 6 This Example illustrates the preparation of 1-trityl-3-bromo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (15.55 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (5.8 g) in dry tetrahydrofuran (500 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (37.5 ml, 1.6M in hexane). The deep-red solution was stirred at -70 C. for twenty minutes, then treated dropwise with a solution of bromine (10.4 g) in dry tetrahydrofuran (10 ml). The now brownish-yellow solution was allowed to warm to -20 C., quenched with 0.1M sodium thiosulphate solution (150 ml), and extracted with dichloromethane (500 ml). The organic layer was washed with water (4*100 ml), dried and evaporated. The residue was chromatographed on silica, using dichloromethane-ether (25:2) as eluant, to give 1-trityl-5-bromo-1,2,4-triazole (7.86 g, m.p. 239-241 C.). NMR (CDCl3):delta7.1-7.3(15H,m), 7.95(1H,s).

I am very proud of our efforts over the past few months and hope to 1-Trityl-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 31250-99-4, New Advances in Chemical Research in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

a) A solution of 1-trityl-1,2,4-triazole (10.0 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (3.8 g) in dry tetrahydrofuran (250 ml) was cooled to -70 C. under nitrogen. n-Butyllithium (22.2 ml, 1.6M solution in hexane) was added dropwise, with stirring, at such a rate that the internal temperature was maintained below -60 C. The red solution was stirred at -70 C. for twenty-five minutes, then treated dropwise with diethyl 3-oxo-propane phosphonate (6.20 g, prepared by formic acid deacetalisation of the diethyl acetal, DE 2517448, and also described in, for example, Tetrahedron 1981, 37, 1377) whilst maintaining the temperature at that level. The mixture was stirred for two and a half hours at -70 C. then quenched, at that temperature, with saturated aqueous ammonium chloride solution. It was extracted with ethyl acetate and the organic phase washed with brine, dried over magnesium sulphate, and evaporated under reduced pressure to give crude diethyl 3-hydroxy-3(1-trityl-1,2,4-triazol-5-yl)propane phosphonate (10.81 g). Chromatography on silica, using dichloromethane-ethanol (19:1) as eluant, gave pure material, m.p. 154-155 C. NMR (CDCl3): delta1.3(6H,t), 1.9(2H,m), 1.7(2H,m), 3.1(1H,br), 4.0(4H,m), 4.1(1H,t), 7.1-7.3 (15H,m), 7.9(1H,s). M/S: M+ 505.

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Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Application of 31250-99-4, New Advances in Chemical Research in 2021. Redox catalysis has been broadly utilized in electrochemical synthesis due to its kinetic advantages over direct electrolysis. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

Triethylamine (5.49 g, 54.30 mmol) is added to a solution of 1,2,4-triazole (3.0 g, 43.44 mmol) in DMF (50 mL) at rt. After stirring for 5 minutes, trityl chloride (12.11 g, 43.44 mmol) is added as a solid and the mixture is stirred overnight. The solvent is distilled off under reduced pressure and the crude is partitioned between dichloromethane (50 mL) and water (50 mL). The organic layer is separated and the aqueous layer is extracted with dichloromethane (3 x 50 mL). The combined organic layers are washed with water (3 x 40 mL). The organic layer is dried over Na2SO4 and concentrated under reduced pressure to afford the product 1-trytil-1H- 1,2,4-triazole (12.6 g, 93 %). n-BuLi (4.5 mL, 11.24 mmol; 2.5 M solution in hexanes) is added to a solution of 1-trityl-1H-1,2,4-triazole (3.5 g, 11.24 mmol) in THF (120 mL) at -78C and the solution is stirred for 45 mm. Bromine (1.76 g, 11.02 mmol) is added dropwise over a period of 5 minutes and the solution is stirred for 2 h allowed to warm to -20 C and quenched by adding saturated NH4C1 solution (30 mL). The reaction mixture ias diluted with water (60 mL) and dichloromethane (40 mL). The organic layer is separated and the aqueous layer is extracted with CH2C12 (4 x 50 mL).The combined organic extract was dried over Na2SO4 and the solvent evaporated under reduced pressure to afford crude which is used as such for the next step (4.2 g, 95 %). 7.09-7.16 (m, 6H), 7.27-7.40 (m, 9H), 7.86 (s, 1H).

I am very proud of our efforts over the past few months and hope to 1-Trityl-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; NEWLINK GENETICS CORPORATION; KUMAR, Sanjeev; WALDO, Jesse; JAIPURI, Firoz; MAUTINO, Mario; WO2014/159248; (2014); A1;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

New discoveries in chemical research and development in 2021. The transformation of simple hydrocarbons into more complex and valuable products via catalytic C–H bond functionalisation has revolutionised modern synthetic chemistry. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole belongs to triazoles compound, it is a common compound, a new synthetic route is introduced below. Formula: C21H17N3

EXAMPLE 4 This Example illustrates the preparation of 1-trityl-5-iodo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (9.95 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (3.71 g) in dry tetrahydrofuran (200 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (22.0 ml, 1.6M solution in hexane). The solution was stirred for ten minutes, then treated rapidly with a solution of iodine (10.0 g) in dry tetrahydrofuran (40 ml). After a further one minute, the mixture was quenched at -50 C. with 0.1M sodium thiosulphate (100 ml) and portioned between dichloromethane and water. The organic layer was washed with water, dried over magnesium sulphate, evaporated under reduced pressure and the residue chromatographed on silica, using dichloromethane-ether (25:2) as eluant to give the title compound (11.73 g, m.p. 248-250 C.). NMR (CDCl3): delta7.1-7.3 (15H,m), 8.0(1H,s). 13 C NMR confirmed position of substitution. M/S: M+ 437

I hope this article can help some friends in scientific research. I am very proud of our efforts over the past few months and hope to 1-Trityl-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Reference of 31250-99-4, New Advances in Chemical Research in 2021. Chemo-enzymatic cascade processes are invaluable due to their ability to rapidly construct high-value products from available feedstock chemicals in a one-pot relay manner. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, below Introduce a new synthetic route.

EXAMPLE 6 This Example illustrates the preparation of 1-trityl-3-bromo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (15.55 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (5.8 g) in dry tetrahydrofuran (500 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (37.5 ml, 1.6M in hexane). The deep-red solution was stirred at -70 C. for twenty minutes, then treated dropwise with a solution of bromine (10.4 g) in dry tetrahydrofuran (10 ml). The now brownish-yellow solution was allowed to warm to -20 C., quenched with 0.1M sodium thiosulphate solution (150 ml), and extracted with dichloromethane (500 ml). The organic layer was washed with water (4*100 ml), dried and evaporated. The residue was chromatographed on silica, using dichloromethane-ether (25:2) as eluant, to give 1-trityl-5-bromo-1,2,4-triazole (7.86 g, m.p. 239-241 C.). NMR (CDCl3):delta7.1-7.3(15H,m), 7.95(1H,s).

I am very proud of our efforts over the past few months and hope to 1-Trityl-1H-1,2,4-triazole help many people in the next few years.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Electric Literature of 31250-99-4, A common heterocyclic compound, 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, 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) A solution of 1-trityl-1,2,4-triazole (10.0 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (3.8 g) in dry tetrahydrofuran (250 ml) was cooled to -70 C. under nitrogen. n-Butyllithium (22.2 ml, 1.6M solution in hexane) was added dropwise, with stirring, at such a rate that the internal temperature was maintained below -60 C. The red solution was stirred at -70 C. for twenty-five minutes, then treated dropwise with diethyl 3-oxo-propane phosphonate (6.20 g, prepared by formic acid deacetalisation of the diethyl acetal, DE 2517448, and also described in, for example, Tetrahedron 1981, 37, 1377) whilst maintaining the temperature at that level. The mixture was stirred for two and a half hours at -70 C. then quenched, at that temperature, with saturated aqueous ammonium chloride solution. It was extracted with ethyl acetate and the organic phase washed with brine, dried over magnesium sulphate, and evaporated under reduced pressure to give crude diethyl 3-hydroxy-3(1-trityl-1,2,4-triazol-5-yl)propane phosphonate (10.81 g). Chromatography on silica, using dichloromethane-ethanol (19:1) as eluant, gave pure material, m.p. 154-155 C. NMR (CDCl3): delta1.3(6H,t), 1.9(2H,m), 1.7(2H,m), 3.1(1H,br), 4.0(4H,m), 4.1(1H,t), 7.1-7.3 (15H,m), 7.9(1H,s). M/S: M+ 505.

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; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Some common heterocyclic compound, 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, molecular formula is C21H17N3, 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. Formula: C21H17N3

EXAMPLE 4 This Example illustrates the preparation of 1-trityl-5-iodo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (9.95 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (3.71 g) in dry tetrahydrofuran (200 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (22.0 ml, 1.6M solution in hexane). The solution was stirred for ten minutes, then treated rapidly with a solution of iodine (10.0 g) in dry tetrahydrofuran (40 ml). After a further one minute, the mixture was quenched at -50 C. with 0.1M sodium thiosulphate (100 ml) and portioned between dichloromethane and water. The organic layer was washed with water, dried over magnesium sulphate, evaporated under reduced pressure and the residue chromatographed on silica, using dichloromethane-ether (25:2) as eluant to give the title compound (11.73 g, m.p. 248-250 C.). NMR (CDCl3): delta7.1-7.3 (15H,m), 8.0(1H,s). 13 C NMR confirmed position of substitution. M/S: M+ 437

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 31250-99-4, its application will become more common.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Synthetic Route of 31250-99-4, 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. 31250-99-4, name is 1-Trityl-1H-1,2,4-triazole, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 6 This Example illustrates the preparation of 1-trityl-3-bromo-1,2,4-triazole. A stirred solution of 1-trityl-1,2,4-triazole (15.55 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (5.8 g) in dry tetrahydrofuran (500 ml) was cooled to -70 C. under nitrogen and treated dropwise with n-butyllithium (37.5 ml, 1.6M in hexane). The deep-red solution was stirred at -70 C. for twenty minutes, then treated dropwise with a solution of bromine (10.4 g) in dry tetrahydrofuran (10 ml). The now brownish-yellow solution was allowed to warm to -20 C., quenched with 0.1M sodium thiosulphate solution (150 ml), and extracted with dichloromethane (500 ml). The organic layer was washed with water (4*100 ml), dried and evaporated. The residue was chromatographed on silica, using dichloromethane-ether (25:2) as eluant, to give 1-trityl-5-bromo-1,2,4-triazole (7.86 g, m.p. 239-241 C.). NMR (CDCl3):delta7.1-7.3(15H,m), 7.95(1H,s).

The chemical industry reduces the impact on the environment during synthesis 1-Trityl-1H-1,2,4-triazole. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 31250-99-4, name is 1-Trityl-1H-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 31250-99-4, Product Details of 31250-99-4

EXAMPLE 2 This Example illustrates the preparation of 1-trityl-1,2,4-triazole-5-carboxaldehyde. A solution of 1-trityl-1,2,4-triazole (62.2 g, prepared as described in Example 1) and N,N,N’,N’-tetramethylethylenediamine (23.2 g, 30 ml) in dry tetrahydrofuran (1 l) was cooled to -70 C. under nitrogen. n-Butyllithium (140 ml, 1.6M solution in hexane) was added dropwise, with stirring, at such a rate that the internal temperature was maintained below -60 C. The dark red solution was stirred at -70 C. for at least thirty minutes, treated dropwise with N,N-dimethylformamide (25 ml), allowed to warm to -30 C., then quenched with water (500 ml). The mixture was extracted with ethyl acetate (500 ml), containing a little dichloromethane if any solid precipitated. The extracts were washed with water (6*500 ml), dried over magnesium sulphate, evaporated under reduced pressure and the crude product triturated with ether-hexane (1:1, 150 ml) to give the title compound (60 g, m.p. 134-136 C.). This can be contaminated with 1,2,4-triazole itself, but subsequent stages are not adversly affected and the impurity can be removed at a later stage. NMR (CDCl3): delta7.1-7.4 (15H,m), 8.1(1H,s), 9.15(1H,s).

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; Zeneca Limited; US5393732; (1995); A;,
1,2,3-Triazole – Wikipedia,
Triazoles – an overview | ScienceDirect Topics