Tag: M.W=100-200

These common heterocyclic compound, 21948-70-9, name is 2-Methylthiopyrazine, 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. Safety of 2-Methylthiopyrazine

General procedure: Under the N2 atmosphere,2x (0.5 mmol) was added to the reaction tube in turn.3b (0.75mmol) and dissolved in 1.0M in advanceThe mixture obtained from KHMDS (0.75 mmol) of THF was heated to 100 C, and the reaction was stirred for about 16 hours until the conversion of the starting material was completed, and the temperature was lowered to room temperature.Diluted with THF (3 ml) to the reaction mixture.Filter through silica gel or diatomaceous earth, wash with THF,The crude product was concentrated in vacuo and subjected to silica gel column chromatography to give the corresponding product 1xb.As shown in the following equation, where, lists the yield of 1xb isolated using different 2x as raw materials.For example, when using 2f?,The yield of the product 1f’b was 88%.

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

Synthetic Route of 89123-58-0, 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. 89123-58-0 name is 5-Bromopyrazine-2,3-diamine, 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.

Example 52A 5-[1-(2-Fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl]pyrazine-2,3-diamine Under argon, 425 mg (1.20 mmol) of the compound from Example 33A were initially charged in 1,4-dioxane (11 ml), and the reaction mixture was purged with argon for 10 min. Thereafter, 0.91 ml (1.80 mmol) of hexabutylditin and 250 mg (1.32 mmol) of 2,3-diamino-5-bromopyrazine were added. Subsequently, 422 mg (0.60 mmol) of bis(triphenylphosphine)palladium(II) chloride were added and the reaction mixture was heated to reflux overnight. Thereafter, the mixture was cooled to RT and filtered through Celite, and the filtrate was concentrated. The residue was admixed with methanol, and the solids were filtered off and discarded. The filtrate was taken up in methanol-dichloromethane, absorbed onto diatomaceous earth and purified on silica gel (eluent: cyclohexane-ethyl acetate 2:1, 1:1). This gave 151 mg (31% purity, 11% of theory) of the title compound. The crude product was converted further without further purification. LC-MS (method 3): Rt=0.91 min MS (ESIpos): m/z=336 (M+H)+

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

Synthetic Route of 1174321-06-2, 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. 1174321-06-2, name is 5-(Difluoromethyl)pyrazine-2-carboxylic acid belongs to pyrazines compound, it is a common compound, a new synthetic route is introduced below.

1) Synthesis of Compound F-21: Compound F-19 (18 mg, 0.04 mmol) was dissolved in dichloromethane (3 mL),1H-benzotriazol-1-yloxytripyrrolidinylhexafluorophosphate (PyBOP) (57 mg, 0.1 mmol), diisopropylethylamine (21.6 muL, 0.13 mmol) was added,5-Difluoromethylpyrazine-2-carboxylic acid (16 mg, 0.09 mmol), reacted overnight at room temperature;TLC showed complete reaction of the raw materials, adding dichloromethane (5mL), and then saturated organic saline to wash the organic phase, the organic phase was dried by spin-drying the column product 23mg;Suggest an edit

The synthetic route of 5-(Difluoromethyl)pyrazine-2-carboxylic acid has been constantly updated, and we look forward to future research findings.

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. 36070-75-4, name is 5-Chloropyrazine-2-carbonitrile, A new synthetic method of this compound is introduced below., Formula: C5H2ClN3

Combine a THJF solution (22%) of fcrt-butyl (3-(2-(2-cyanoacetyl)-3- memoxyphenoxy)propyl)carbamate (1.0 eqv, this is define as one volume) with hydrazine (35%, 1.5 eqv), acetic acid (glacial, 1.0 eqv), water (1 volume based on the THF solution) and methanol (2 volumes based on the THF solution). This is a continuous operation. Heat the resulting mixture to 130 C and 1379 kPa with a rate of V/Q = 70 minutes, tau = 60. Extract the solution with toluene (4 volumes), water (1 volume), and sodium carbonate (10% aqueous, 1 eqv). Isolate Ihe toluene layer and add to DMSO (0.5 volumes). Collect a solution of the intermediate compound tert-butyl (3-(2-(3-amino-lH- pyrazol-5-yl)-3-methoxyphenoxy) propyl)carbamate (26.59 kg, 91%) in 10 days, mp = 247.17 C as a DMSO solution (3 volumes of product). N-Eftylmorpholine (1.2 eqv) and 5-chloropyrazine-2-carbonitrile (1.15 eqv) in 2 volumes of DMSO is combined in a tube reactor at 80 C, V/Q = 3 and tau = 170 minutes at ambient pressure. Add the product stream to methanol (20 vol). As a continuous process, filter the mixture and wash with methanol followed by MTBE. Air dry the material on the filter to give tert-butyl (3-(2- (3-((5-cyanopyrazm-2-yl)arnino)-lH-pyrazol-5-yl)-3-methox>’phenoxy) propyl)carbamate in a continuous fashion (22.2 kg, 88.7%, 8 days). Dissolve a solution of fcrt-butyl (3-(2- (3-((5-cyanopyrazin-2-yl)amino)-lH-pyrazol-5-yl)-3-methoxyphenoxy) propyl)carbamate in formic acid (99%, 142 kg) at ambient temperature and agitate for 4 hours to provide an intermediate of 5-((5-(2-(3-aminopropoxy)-6-methoxyphenyl)-lH-pyrazol-3- yl)amino)pyrazine-2-carbonitrile formate. Dilute the solution with water (55 kg), (S)- lactic acid (30%, 176 kg) and distill the resulting mixture until 10% relative humidity to give the title product as a white to yellow solid (24.04 kg, 85-90%), mp. 157 C.

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.

Application of 4774-14-5,Some common heterocyclic compound, 4774-14-5, name is 2,6-Dichloropyrazine, molecular formula is C4H2Cl2N2, 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 solution of compound 8 (450.0 g, 3.02 mol) in cone. aq. NH3 (3.0 L) was stirred at 135C overnight in a 10 L sealed pressure vessel. TLC and LC/MS showed complete conversion of the starting material. The reaction mixture was cooled to room temperature and filtered to afford a white solid. The solid was washed with water (200 mL x 3), and then dried to afford compound 9 (312 g, 80% yield) as a solid. 1HNMR (400 MHz, DMSO- 6): delta 7.82 (s, 1 H), 7.12 (s, 1 H), 6.93 (s, 2H). MS Calcd.: 129 MS Found: 130 ([M+H]+).

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

Application of 1111638-10-8, 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 1111638-10-8 as follows.

To a solution of 3-chloro-5H-pyrrolo[2,3-b ]pyrazine (300 mg, 1.95 mmol) in2-methyltetrahydrofuran (10 mL) was added NIS (543 mg, 2.34 mmol), and the reaction mixturewas stirred at rt for 1 h. Saturated aqueous sodium thiosulfate (50 mL) was added to quench thereaction, and the resulting mixture was partitioned. The aqueous layer was extracted with EtOAc(50 mL x 2). The combined organic phases were washed with saturated brine (80 mL), driedover anhydrous Na2S04, filtered, and the filtrate was concentrated in vacuo to give the titlecompound as a yellow solid (546 mg, 100 %).MS (ESI, pos. ion) m/z: 280.2 [M+Ht.

According to the analysis of related databases, 1111638-10-8, the application of this compound in the production field has become more and more popular.

Related Products of 55557-52-3, 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. 55557-52-3 name is 3-Chloropyrazine-2-carbonitrile, 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.

2-Cyano-3-chloropyrazine (1.5 g, 10.8 mmol) and Raney-Ni (50% slurry in water, 0.5 g) were added to 15 mL of glacial acetic acid under nitrogen for three times.Stir at 50 C overnight under a hydrogen atmosphere of 3 atm. After the reaction is complete, it is filtered.The filtrate was concentrated and the residue dissolved in ethyl acetate.Dry over anhydrous sodium sulfate, concentrate,The pale yellow oil was separated by a silica gel column (0.82 g).The yield was 53%.

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

Reference of 21279-62-9, 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. 21279-62-9 name is 3-Chloropyrazine-2-carboxamide, 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.

General procedure: Compounds 1-6 were prepared according to conventional organic synthesis methods. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was dissolved in THF (20 mL) in a round bottom flask and after that treated with two equivalents of the corresponding benzylamine and an equimolar amount of triethylamine. The reaction was conducted with continuous stirring and heating (70 C) under reflux in an oil bath for 15 h. Compounds 7-15 were synthesised using a microwave reactor with a focused field. 3-Chloropyrazine-2-carboxamide (1.27 mmol) was put into a thick-walled tube together with the corresponding benzylamine (2.54 mmol), pyridine (1.27 mmol), methanol (approx. 5 mL) and a magnetic stir bar and then sealed with a special cap. The reaction parameters were set according to the previously published paper as follows-140 C, 30 min, 200 W [29]. Reaction progress was checked by TLC (hexane:ethyl acetate-1:1). Regardless of the synthesis method used,all reaction mixtures were adsorbed on silica and subjected to preparative flash chromatography (hexane and ethyl acetate, gradient elution, detection wavelengths 260 nm and 280 nm). Products were recrystallized from ethanol or ethanol and water if necessary. All final substances were chemically characterized (1H-NMR, 13C-NMR, IR, melting point and elemental analysis).

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

Synthetic Route of 5780-66-5,Some common heterocyclic compound, 5780-66-5, name is Pyrazine-2-carbaldehyde, molecular formula is C5H4N2O, 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.

As shown in scheme 1, nitromethane (11.1 mL, 207 mmol, 1.5 eq) was added to a solution of the pyrazine aldehyde (15 g, 138 mmol) in 35 mL of anhydrous THF. The solution was cooled to 0° C. Potassium tert-butoxide (13.8 mL of 1 M solution in THF, 13.8 mmol, 0.1 eq) was added dropwise keeping the solution temperature below 5° C. A yellow precipitate formed upon addition of base. After addition of base was complete, the reaction was stirred for 15 minutes at 0° C. The solution was poured into 250 mL of water and extracted with EtOAc (3.x.250 mL). The combined organics were washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified via silica plug and eluted with 60percent EtOAc/hexanes. The product (1) was a yellow viscous oil (15.1 g, 64percent). LC/MS (M+1) 170.

The synthetic route of 5780-66-5 has been constantly updated, and we look forward to future research findings.

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 54608-52-5 as follows. Recommanded Product: 54608-52-5

General procedure: p-TsOH (9.5 mg, 55 mumol, 5 mol %) and MnO2 (348 mg, 4.00 mmol) were added to a stirred solution of heterocyclic hydrazine 1a-d (1 mmol) and aldehyde 2a-k (1.2 mmol) in PhMe (10 ml). The mixture was heated at 80C until the starting material was completely consumed (monitored by TLC, 40-55 min) and then cooled down to room temperature. After filtration and evaporation of solvent from the filtrate, the resulting residue was purified by silica gel column chromatography affording pure products.

According to the analysis of related databases, 54608-52-5, the application of this compound in the production field has become more and more popular.