Month: April 2021

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. 762240-92-6, name is 3-(Trifluoromethyl)-5,6,7,8-tetrahydro-[1,2,4]triazolo[4,3-a]pyrazine hydrochloride, A new synthetic method of this compound is introduced below., COA of Formula: C6H8ClF3N4

Into a 50 mL round-bottom flask was added 20 mL acetonitrile, followed by the addition of the phenyl-butyric acid derivative obtained in Example 46 (3.32 g, 0.01 mol) and triazolopyrazine hydrochloride (228 g, 0.01 mol). The temperature of the reaction mixture was cooled down to 0 C. in an ice-salt bath. 1-Hydroxylbenzotriazole (1.62 g, 0.012 mol) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.29 g, 0.012 mol) were further added. 3 g Triethylamine was then added dropwise and the mixture was stirred at room temperature for 24 h. The reaction solution was washed with 3 X 20 mL distilled water. The obtained organic layers were collected and dried over anhydrous magnesium sulfate for 1 h. Then, the desiccant was filtered off and the resulting reactant was concentrated to 4.81 g. The yield was 95%. [alpha] D20=+22.2 (c 1.0, CHCl3). M.p. 188-191 C. IR (cm-1): 3374, 2897, 1686, 1635, 1519, 1368, 1164, 1128, 1016. 1H NMR (400 MHz, CDCl3) delta 7.187.05 (m, 1H), 7.02-6.85 (m, 1H), 5.31 (s, 1H), 5.154.76 (m, 2H), 4.433.78 (m, 5H), 2.982.92 (m, 2H), 2.712.61 (m, 2H), 1.36 (s, 9H). ESI-MS: 508.0 (M++1). HRMS Calcd. for: C21H23F6N5O3Na (M+Na)+ requires 530.1598, found 530.1604.

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.

Related Products of 41110-33-2, 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. 41110-33-2 name is Methyl 5-methylpyrazine-2-carboxylate, 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.

[0115j To a solution of methyl 5-methylpyrazine-2-carboxylate (0.5 g, 3.28 mmol) in acetic acid (5 ml) was added bromine (0.i9 ml, 3.6i mmol) at room temperature. The reaction mixture was heated at 80C for 45 mm. The reaction mixture was concentrated to remove acetic acid. The residue was basified with saturated sodium bicarbonate solution and extracted with ethyl acetate. The organic layer was dried and concentrated. The crude was purified by silica gel column chromatography using 20% ethyl acetate in hexane to afford the title compound methyl 5-(bromomethyl)pyrazine-2-carboxylate (0.3 g, 40%) as a brownish liquid. Calculated M+H: 230.97; Found M+H: 231.0.

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

Related Products of 5521-55-1, 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. 5521-55-1 name is 5-Methylpyrazine-2-carboxylic acid, 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 250 ml four-necked flask was added 13.8 g of 5-methylpyrazine-2-carboxylic acid and 35.7 g of thionyl chloride, and the mixture was heated with stirringReflux reaction 2h, stop heating, vacuum distillation out of excess thionyl chloride, to be evaporated to dry, cooled to room temperature. The residue is dissolved138 g of dichloromethane, and then 20.4 g of p-aminoethylbenzenesulfonamide was added, and 30.4 g of triethylamine was slowly added with stirring,And then stirred at room temperature for 12 h. Filter, and with a small amount of dichloromethane rinse, dry, the filter cake into the water, with hydrochloric acidPH = 1, stirring for 20min, filtered and washed with water to neutral, the resulting solid at 60 ~ 70 for 12h, you can get29.5 g of a white solid product, 2- [4-aminosulfonyl-phenyl] -ethyl-5-methylpyrazine formamide, yield 92.2%.

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

Reference of 5049-61-6, A common heterocyclic compound, 5049-61-6, name is Pyrazin-2-amine, molecular formula is C4H5N3, 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.

Method b:; 2-Amino-pyrazine (0.10 g, 1.05 mmol) and NCS (80 mg, 0.60 mmol) were added in a microwave tube with 1.5 mL of the anhydrous CHCl3 and sealed. The tube was placed in the microwave cavity and heated at 70C for 10 min. (70C10M60W300Psi). After the workup, the crude (0.15 g) was purified by FCC (Hexane/DCM/ AcOEt = 1 :1 :1) to afford 35 mg (yield 45%) of the product as yellow solid. 1H NMR (270 MHz; d6-DMSO), delta 7.99 (IH, s, H-6), 7.67 (IH, s, H-3), 6.65 (2H, bs, NH2). m/z (EI-MS): 129 (M+), 99, 94 ([M-Cl]+).; When the distilled chloroform used for the reaction was pre-treated over basic Al2O3, the black polymers formed in the reaction decreased dramatically. When NCS was added slowly into the refluxing 2-aminopyrazine, the product was isolated at 26%. Moreover, when microwave irradiation was used at 70C for 10 min., the yield reached 45% (Figure 4)

The synthetic route of 5049-61-6 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 5049-61-6, A common heterocyclic compound, 5049-61-6, name is Pyrazin-2-amine, molecular formula is C4H5N3, 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 250ml round bottom flask was charged with 2-aminopyrazine (1Og, O.lmol), N-chlorosuccinimide (14g, O.lmol) and dichloromethane (100ml) under nitrogen. The reaction mixture was refluxed for 5h, then allowed to cool to room temperature. The reaction mixture was filtered though a 1 cm thick celite pad, which was then thoroughly washed with dichloromethane. The EPO organic was concentrated in vacuo and the compound was purified by flash chromatography, using as eluent pentane/EtOAc 0% to 50%, to give the title compound (3g, 22%). IHNMR (CDCl3) 4.5-4.8 (2H, brs), 7.8 (IH, s), 8.0 (IH, s).

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.

Related Products of 939412-86-9, The chemical industry reduces the impact on the environment during synthesis 939412-86-9, name is (3-Chloropyrazin-2-yl)methanamine hydrochloride, I believe this compound will play a more active role in future production and life.

To a stirred suspension of (3-chloropyrazin-2-yl)methanamine hydrochloride (0092) (500 mg, 2.78mmol) in ethyl acetate (10 mL) was added acetic anhydride (315 pL, 3.33 mmol) dropwise, followed by triethylamine (1.16 mL, 8.34 mmol). The mixture was stirred at room temperature for 1 h, and the solvent was removed under reduced pressure. The obtained residue was dissolved in methylene chloride (150 mL) and washed with saturated NaHC03 (2 c 25 mL). The organic phase was evaporated under reduced pressure and was further dried under high vacuum to give the title compound as a beige solid (376 mg, 72.9% yield), which was directly used for the next reaction without further purification. MS (ESI) m/z 186.0507 [M + H]+. 1H NMR (500 MHz, Chloroform-d) d 8.5 (d, J = 2.51 Hz, 1H), 8.3 (d, J = 2.55 Hz, 1H), 4.7 – 4.7 (m, 2H), 2.1 (s, 3H)).

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, (3-Chloropyrazin-2-yl)methanamine hydrochloride, other downstream synthetic routes, hurry up and to see.

Electric Literature of 6966-01-4, These common heterocyclic compound, 6966-01-4, name is Methyl 3-amino-6-bromopyrazine-2-carboxylate, 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.

To a 250 ml reaction flask add 43g III, 43 ml 98.3% concentrated sulfuric acid, stirring. – 20 – 0 C lower, adding 25.6g sodium nitrite, canada finishes rose to 55 – 60 C, thermal insulation stirring for about 30min to the raw basic reaction end. The reaction liquid dropping 430g ice water, canada finishes insulation stirring for about 1.5h to the reaction is complete. Filtering, the filter cake 50 C drying by blowing 6h, get 37.6g orange solid IV, yield 87%.

The synthetic route of 6966-01-4 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. 5521-55-1, name is 5-Methylpyrazine-2-carboxylic acid, A new synthetic method of this compound is introduced below., Product Details of 5521-55-1

A mixture of 5-methyl-2-pyrazinecarboxylic acid (1) (0.01 mol) and hydrazine hydrate (0.025 mol) in ethanol (20 mL) was refluxed for 9 h on consistent stirring. After completion of the reaction (monitored by the TLC), the reaction mixture is cooled to room temperature, poured in ice-cold water (20 mL). Thus the solid separated was filtered off and the crude product was recrystallized from ethyl acetate to give pure 5-methyl-2-pyrazinecarboxylic acid hydrazide (2).

The synthetic route of 5521-55-1 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 356783-16-9, name is 3,6-Dichloropyrazine-2-carbonitrile, 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. Recommanded Product: 3,6-Dichloropyrazine-2-carbonitrile

REFERENTIAL EXAMPLE II-15 In 50 mL of N,N-dimethylformamide was dissolved 10.0 g of 3,6-dichloro-2-pyrazinecarbonitrile. After adding 6.49 mL of thiophenol and 11.91 g of potassium carbonate successively, the mixture thus obtained was stirred at 40 C. for 3 hours. The reaction mixture was poured into a mixture of 100 mL of ethyl acetate and 100 mL of water, and pH was adjusted to 2 with 6 mol/L hydrochloric acid. The organic layer was separated, washed successively with water and saturated aqueous solution of sodium chloride, and dried on anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent: toluene:n-hexane=1:3] to obtain 3.80 g of 6-chloro-3-(phenylsulfanyl)-2-pyrazinecarbonitrile as a light yellow-colored oily product. R (neat) cm-1: 2238 H-NMR (CDCl3) delta: 7.00-7.70(5H,m), 8.39(1H,s)

The synthetic route of 3,6-Dichloropyrazine-2-carbonitrile has been constantly updated, and we look forward to future research findings.

Synthetic Route of 143591-61-1,Some common heterocyclic compound, 143591-61-1, name is 3-Bromo-8-chloroimidazo[1,2-a]pyrazine, molecular formula is C6H3BrClN3, 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.

Intermediate Example 3-1 : Preparation of 3-bromo-8-methylsulfanyl- imidazo[1 ,2-a]pyrazine To a stirred solution of 3-bromo-8-chloro-imidazo[1 ,2-a]pyrazine ( 1 1 .63 g, 50 mmol) in 120 mL NMP is added at -15C under stirring sodium thiomethylate (3.52 g, 50 mmol) After stirring for 4 h the mixture is left to come to rt and stirred overnight. 500 mL of water are added and the light brown solid is filtered off, washed and dried in vaccuo to yield 8.81 (72 %) of the title compound. UPLC-MS: RT = 0.93 min; m/z 245.1 [MH+]; required MW = 244.1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromo-8-chloroimidazo[1,2-a]pyrazine, its application will become more common.