Month: April 2021

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 14508-49-7 as follows. Safety of 2-Chloropyrazine

A mixture of 2-hydrazinopyrazine (820 mg, 7.45 mmol), prepared from 2-chloropyrazine and hydrazine using a procedure analogous to that described in the literature (P. J. Nelson and K. T. Potts, J. Org. Chem. 1962, 27, 3243, except that the crude product was extracted into 10% methanol/dichloromethane and filtered, and the filtrate was concentrated and purified by flash chromatography on silica gel, eluting with 100% ethyl acetate followed by 10% methanol in dichloromethane), TFA (2.55 g, 22.4 mmol), and polyphosphoric acid (10 mL) was heated to 140 C. with stirring for 18 h. The solution was added to ice and neutralized by the addition of ammonium hydroxide. The aqueous solution was extracted with ethyl acetate (3×), washed with brine, and dried over anhydrous magnesium sulfate. Concentration followed by flash chromatography (silica gel, 1:1 hexane:ethyl acetate, then 100% ethyl acetate) afforded the title compound as a solid (861 mg). 1H NMR (500 MHz, CDCl3) delta 8.17-8.20 (m, 2H), 9.54 (s, 1H). LC/MS (M+1) 189.

According to the analysis of related databases, 14508-49-7, the application of this compound in the production field has become more and more popular.

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. 912773-21-8, name is 2-Bromo-5-chloropyrazine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 912773-21-8

Intermediate 30a and 30b: N-[(1S,2S)-2-[(5-Bromopyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Intermediate 30a) and N-[(1S,2S)-2-[(5-Chloropyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Intermediate 30b) A solution of N-[(1S,2S)-2-aminocyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide hydrochloride (Intermediate 4; 1.00 g, 3.25 mmol), 2-bromo-5-chloropyrazine (CAS number 912773-21-8; 0.691 g, 3.57 mmol) and DIPEA (1.7 ml, 9.75 mmol) in DMSO (11 ml) was subjected to microwave irradiation at 140 C. for 3 hours. The reaction was partitioned between ethyl acetate and water, washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. This was then purified by column chromatography (silica, 0-100% ethyl acetate/petrol then 0-20% methanol ethyl acetate) to afford title compound as a mixture of both products Example 112 N-[(1S,2S)-2-[(5-Cyclopropylpyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide A mixture of N-[(1S,2S)-2-[(5-bromopyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide and N-[(1S,2S)-2-[(5-chloropyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Intermediate 30a and 30b; 100 mg, 0.23 mmol), cyclopropylboronic acid (CAS number 411235-57-9; 60 mg, 0.70 mmol), sodium carbonate (aq. 2 M, 350 mul, 0.70 mmol) and tetrakis(triphenylphosphine)palladium (27 mg, 0.023 mmol) in 1,4-dioxane (778 mul) was sealed, purged and evacuated with nitrogen and then subjected to microwave irradiation at 100 C. for 1 hour. To this was then added further cyclopropylboronic acid (CAS number 411235-57-9; 60 mg, 0.70 mmol) and tetrakis(triphenylphosphine)palladium (27 mg, 0.023 mmol). The reaction was sealed, purged and evacuated with nitrogen and again subjected to microwave irradiation at 140 C. for 20 minutes. The reaction was partitioned between ethyl acetate and water, washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol) and then purified by reverse phase preparative HPLC (eluted with acetonitrile/water containing 0.1% formic acid) and further purified by column chromatography (basic silica, 0-100% ethyl acetate/petrol) to afford the title compound. 1H NMR (400 MHz, DCM-d2) delta ppm 0.77-0.92 (m, 4H), 1.40-1.60 (m, 2H), 1.68-1.94 (m, 3H), 2.14-2.29 (m, 2H), 3.80-3.91 (m, 1H), 3.99-4.10 (m, 1H), 6.65-6.73 (m, 1H), 7.43-7.59 (m, 4H), 7.64 (s, 2H), 7.68-7.72 (m, 1H), 7.74-7.78 (m, 1H) and 7.84 (br. s., 1H). MS ES+: 390 Example 113 N-[(1S,2S)-2-{[5-(Propan-2-yl)pyrazin-2-yl]amino}cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide Prepared according to the procedure for N-[(1S,2S)-2-[(5-cyclopropylpyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Example 112) from N-[(1S,2S)-2-[(5-bromopyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide and N-[(1S,2S)-2-[(5-chloropyrazin-2-yl)amino]cyclopentyl]-2-(2H-1,2,3-triazol-2-yl)benzamide (Intermediate 30a and 30b; 100 mg, 0.23 mmol) and 4,4,5,5-tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane (CAS number 126726-62-3; 165 mg, 0.98 mmol) except this was purified only by column chromatography (silica, 0-100% ethyl acetate petrol) and then was dissolved in ethanol (2.5 ml). To this was then added palladium on carbon (10% wt, 50% wet) (26 mg, 0.025 mmol) and the resulting mixture was stirred under a balloon of hydrogen gas for 2 hours. The reaction was filtered through diatomaceous earth (commercially sold under the trade mark ?Celite?) and concentrated in vacuo. This was purified by column chromatography (basic silica, 0-100% ethyl acetate petrol) to afford the title compound. 1H NMR (400 MHz, DMSO-d6) delta ppm 1.13-1.20 (m, 6H), 1.37-1.57 (m, 2H), 1.58-1.72 (m, 2H), 1.93-2.07 (m, 2H), 2.81-2.91 (m, 1H), 3.95-4.09 (m, 2H), 6.72-6.78 (m, 1H), 7.40-7.44 (m, 1H), 7.46-7.51 (m, 1H), 7.57-7.62 (m, 1H), 7.75-7.78 (m, 1H), 7.80-7.82 (m, 1H), 7.92-7.93 (m, 1H), 7.94 (s, 2H), 8.35-8.39 (m, 1H). MS ES+: 392

According to the analysis of related databases, 912773-21-8, the application of this compound in the production field has become more and more popular.

Electric Literature of 36070-80-1, The chemical industry reduces the impact on the environment during synthesis 36070-80-1, name is 5-Chloropyrazine-2-carboxylic acid, I believe this compound will play a more active role in future production and life.

General procedure: A solution of compound 10 (216 mg, 1.36 mmol)in SOCl2 was heated to reflux overnight. The excess SOCl2 wasremoved by vacuum distillation. The residue was dissolved in CH2-Cl2 and carefully treated with a solution of 2-amino-6-methylpiridine(739 mg, 6.83 mmol) and NEt3 (275 mg, 2.7 mmol) in CH2Cl2.The mixture was stirred at rt overnight. After the reaction wascompleted, the mixture was extracted with CH2Cl2, washed withwater, brine, and dried over Na2SO4. The organic phase was concentratedin vacuo and the residue was recrystallized from 2-propanolto give compound 11a as a yellow solid (181 mg, 53%).

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, 5-Chloropyrazine-2-carboxylic acid, other downstream synthetic routes, hurry up and to see.

14508-49-7, name is 2-Chloropyrazine, belongs to pyrazines compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C4H3ClN2

EXAMPLE 1; [5-(5-{4-[(2-Bromo-5-fluorophenyl)carbonyl1piperazin-l-yl}pyrazin-2-yl)-2i/-tetrazol-2- yl] acetic acid; Step 1 : fert-Butyl 4-(pyrazin-2-yl)piperazine- 1 -carboxylate; Into a 1 L flask equipped with a condenser and a magnetic stir bar was added 2- chloropyrazine (20.6 g, 180 mmol), tert-buXyl piperazine-1-carboxylate (33.5 g, 180 mmol), potassium carbonate (29.8 g, 216 mmol), dioxane (225 mL) and DMF (225 mL). The mixture was heated to 120 0C for 3 days. The mixture was cooled and poured into a 1 L separatory funnel containing brine (600 mL) and extracted with Et2O (3 x 200 mL). The combined organic layers were washed with brine, dried over MgSO4, filtered and concentrated under reduced pressure. Purification by column chromatography through silica gel, eluting with 50:50 hexanes:EtOAc to 20:80 hexanes:EtOAc as a gradient, afforded the title compound as a yellow solid.

The synthetic route of 14508-49-7 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 63286-28-2, name is 2-Chloro-3-hydrazinylpyrazine, belongs to pyrazines 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 63286-28-2, name: 2-Chloro-3-hydrazinylpyrazine

To a solution of commercial available 2-chloro-3-hydrazinylpyrazine (28 g, 0.19 mol) in dichloromethane (200 mL) was added butyraldehyde (14.7 g, 0.20 mol) and the reaction was stirred at 50 C for 2 hours before cooling to 0 C. Diacetoxyiodobenzene (71 .8 g, 0.223 mol) was added at 0 C. Cooling was removed and the mixture was stirred at 20C for 2 hours. A saturated aq. solution of Na2CO3 (80ml_) was slowly poured into the reaction and the mixture was stirred for 10 minutes. The organic phase was separated, washed with brine (3^50 mL), dried over Na2SO4 and concentrated under vacuum. The residue was purified by flash chromatography on silica gel using a gradient of ethyl acetate and petroleum ether to give 8-chloro-3-propyl-[1 ,2,4]triazolo[4,3-a]pyrazine 20 g (53%) .

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.

These common heterocyclic compound, 75907-74-3, name is (3,5,6-Trimethylpyrazin-2-yl)methanol, 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. name: (3,5,6-Trimethylpyrazin-2-yl)methanol

Reaction step 2-hydroxymethyl-3,5,6-trimethylpyrazine (9.5 g, 62.5 mmol) was sequentially added to a 250 mL three-necked flask,MnO2 (16.2 g, 187.5 mmol),Ethanol 100mL,Reflux 12h,TLC (petroleum ether – ethyl acetate 2: 1) detection reaction is almost complete,cool down,Filtering to obtain filtrate,Ethanol recovery under reduced pressure,To give a yellow solid,Purification by silica gel column chromatography (petroleum ether-ethyl acetate 4: 1)3,5,6-trimethylpyrazine-2-carbaldehyde as a pale yellow solid,The yield was 93.9%

The synthetic route of (3,5,6-Trimethylpyrazin-2-yl)methanol has been constantly updated, and we look forward to future research findings.

Related Products of 32974-92-8, 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. 32974-92-8, name is 1-(3-Ethylpyrazin-2-yl)ethanone belongs to pyrazines compound, it is a common compound, a new synthetic route is introduced below.

(1) Dissolving 10 mmol of 2-acetyl-3-ethylpyrazine in 20 mL of methanol,Stir at 60 C for 15 min,Then 20mL, 10mmol4-methylthiosemicarbazideMethanol solution is added dropwiseInto the above solution,After refluxing at 60 C for 12 h,After cooling to room temperature, pour into the beaker and evaporate.The pale yellow crystal obtained above was filtered and washed with methanol three times.Get ligand (L2);

The synthetic route of 1-(3-Ethylpyrazin-2-yl)ethanone has been constantly updated, and we look forward to future research findings.

4774-14-5, name is 2,6-Dichloropyrazine, belongs to pyrazines compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Recommanded Product: 2,6-Dichloropyrazine

To a solution of 2, 6-dichloropyrazine (50 mg, 0.34 mmol) in DMF (1 mL) was added a solution of potassium cyanide (24 mg, 0.37 mmol) in H20 (1 mL). After stirring for 3 h at 100 C, the reaction mixture was cooled to r. T., poured into H20 (10 mL) and extracted with EtOAc three times. The combined organic layer was dried over MGS04, filtered and concentrated. The crude product wa purified by column chromatography (silica gel, EtOAc: Hexane, 3: 7) to give 15 mg of the desired product. Yield: 32%. 20. 1. a 6-CLALOROPVRAZINE-2-CARBOXYLIC ACID AMIDE MS M/Z 158.1 (M + 1).

The synthetic route of 4774-14-5 has been constantly updated, and we look forward to future research findings.

Related Products of 2727-13-1, 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. 2727-13-1, name is 3-Amino-6-chloropyrazine-2-carboxylic acid belongs to pyrazines compound, it is a common compound, a new synthetic route is introduced below.

To a mixture of 3-amino-6-chloropyrazine-2-carboxylic acid (1.00 g; 5.76 mmol) and triethylamine (2.40 ml; 17.3 mmol) in abs. DMF is added 2-tert-butyl-5-methyl-1,2-oxazol-2-ium hexafluoro-phosphate (4.93 g; 17.3 mmol). The mixture is stirred at r.t. over night. Ice-water is added. The supernatant is decanted from the resin-like product which is sufficiently pure to be further reacted (C13H17ClN4O3) ESI Mass spectrum: m/z=313 [M+H]+

The synthetic route of 3-Amino-6-chloropyrazine-2-carboxylic acid has been constantly updated, and we look forward to future research findings.

Synthetic Route of 486460-21-3, 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 486460-21-3 as follows.

Example 22: Preparation of ((R)-3-(methoxyamino)-1-(3-(trifluoromethyl)-5,6-dihydro-[1,2,4]triazolo[4,3-a]pyrazin-7(8H)-yl)-4-(2,4,5-trifluorophenyl)butan-1-one (formula 16, R2=OMe) [Show Image] 6.0 g of compound of formula 15, 0.3 g 1-hydroxybenzotrizole hydrate (HOBt) and 4.7 g 3-(trifluoro-methyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazine were dissolved in 40 mL of dry dichloromethane. To the clear solution 4.5 mL of N,N’-diisopropylcarbodiimide were added during stirring at 20 C. After addition, the reaction mixture was kept stirring for 2 hours at 23 C, followed by cooling the reaction mixture to 0 C for 2 hours. The precipitate was filtered-off and discarded. The filtrate was evaporated at 45 C and 5 mbar of final pressure, obtaining 12.0 g of crude product.

According to the analysis of related databases, 486460-21-3, the application of this compound in the production field has become more and more popular.