Month: May 2021

Electric Literature of 288-32-4, A common heterocyclic compound, 288-32-4, name is 1H-Imidazole, molecular formula is C3H4N2, 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.

General procedure: Arylhalide (1.0 mM), nitrogen-containing heterocycle (1.2 mM), KOH (2 mM), and the catalyst (0.75 M%) were stirred in dimethyl sulfoxide (DMSO) (4 mL) at 110 C for 10 h. After completion of the reaction, the mixture was cooled to room temperature, diluted with ethyl acetate (10 mL) and filtered. The filtrate was concentrated and the residue was purified by column chromatography on silica gel using hexane/ethyl acetate(70 : 30) as eluent to afford the desired product. The products have been characterized by 1H NMR spectroscopy.

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.

Adding a certain compound to certain chemical reactions, such as: 3034-50-2, name is Imidazole-4-carbaldehyde, belongs to imidazoles-derivatives 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 3034-50-2, name: Imidazole-4-carbaldehyde

To a stirring solution of NaH (1.25 g, 52.1 mmol) in DMF (65 mL) was added SM1 (5 g, 52.1 mmol) followed by iodomethane (8.13 g, 57.3 mmol) at 0 C. Thereaction mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with water and extracted with DCM. Combined organic extracts were dried over anhydrous Na2SO4 and concentrated under reduced pressure to obtain crude product, which was purified by silica gel column chromatography eluting with 5% MeOH/ DCM to compound 1(1.95 g, 34%) as a yellow solid. LC-MS: m/z = 111[(M+1)].

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, Imidazole-4-carbaldehyde, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 3304-70-9, name is Dimethyl 4,5-imidazoledicarboxylate, belongs to imidazoles-derivatives 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 3304-70-9, Quality Control of Dimethyl 4,5-imidazoledicarboxylate

At ambient temperature 9.50 g (59.45 mmol) bromine were added dropwise to a solution of 9.90 g (53.76 mmol) dimethyl imidazole-4,5-dicarboxylate in 300 ml dichloromethane and 80 ml acetonitrile. 7.46 g (54.00 mmol) potassium carbonate was added, and the reaction mixture was stirred for 2 hours at ambient temperature. Then the dichloromethane was eliminated using the rotary evaporator and the residue was combined with a saturated solution of sodium chloride and sodium thiosulphate. It was extracted ten times with ethyl acetate, the organic extracts were dried over sodium sulphate and then the solvent was eliminated. Yield: 12.31 g (87% of theory) C7H7BrN2O4 (263.05) Mass spectrum: (M+H)+=263/265 (bromine)

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, Dimethyl 4,5-imidazoledicarboxylate, other downstream synthetic routes, hurry up and to see.

Reference of 17325-26-7, 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. 17325-26-7, name is Methyl 1H-imidazole-5-carboxylate belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a stirred solution of (S)-2-((4-iodopyridin-2-yl)amino)butan-1-ol (0.8 g, 1.71 mmol), in DMF (5 mL) was added potassium phosphate (0.32 g, 2.57 mmol), methyl 1H-imidazole-4-carboxylate (0.323 g, 2.57 mmol), and L-proline (0.039 g, 0.34 mmol). The mixture was degassed with argon gas for 20 min, then copper(I) iodide (0.065 g, 0.34 mmol) was added, and then the mixture was stirred for 12 h at 150 C. in a sealed glass tube. Then the reaction mixture was cooled and quenched with water (35 mL), and extracted with ethyl acetate (3×60 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated under reduced pressure, and the residue was purified by gradient column chromatography eluting with 80% ethyl acetate in n-hexane to give (S)-methyl 1-(2-((1-hydroxybutan-2-yl)amino)pyridin-4-yl)-1H-imidazole-4-carboxylate as an off-white semi-solid, (0.25 g, 32% yield). 1HNMR (400 MHz, DMSO-d6): delta 8.42 (s, 1H), 8.38 (s, 1H), 8.02 (d, J=6 Hz, 1H,), 7.67 (m, 1H), 6.85 (m, 1H), 6.75 (s, 1H), 6.36 (d, J=8.4 Hz, 1H), 5.72 (s, 1H), 4.61 (s, 1H), 4.12 (m, 1H), 3.81 (d, J=4 Hz, 1H), 3.78 (s, 3H), 3.46 (t, J=5.6 Hz, 1H), 3.34 (t, J=5.6 Hz, 2H), 1.60-1.44 (m, 1H), 1.33-1.24 (m, 1H), 0.89-0.83 (m, 3H). LC-MS calcd exact mass 290.14, found m/z 291.2 [M+H]+.

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, Methyl 1H-imidazole-5-carboxylate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 152628-02-9,Some common heterocyclic compound, 152628-02-9, name is 1,7′-Dimethyl-2′-propyl-1H,1’H-2,5′-bibenzo[d]imidazole, molecular formula is C19H20N4, 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.

In a container equipped with a thermometer, a stirrer, and a condenser, 2-n-propyl-4-methyl-6- (1?-methylbenzimidazol-2-yl) benzimidazole (purity 94.4%) 30. 0 part by weight and 124 parts by weight of N-methyl-2-pyrrolidone were charged and dissolved at 20-25 C. with stirring. Next, 11.1 parts by weight of t-butoxypotassium was charged at 20-30 C. over about 30 minutes, and then cooled to 2-5 C.In this mixed solution, 124 parts by weight of N-methyl-2-pyrrolidone and 33.1 parts by weight of 4?-bromomethylbiphenyl-2-carboxylic acid methyl ester were charged and dissolved at 15 to 20 C. with stirring. The total amount of 157.1 parts by weight of N-methyl-2-pyrrolidone solution containing 4?-bromomethylbiphenyl-2-carboxylic acid methyl ester was added dropwise over a period of 30 minutes in the range of 2 to 5 C. The mixture was kept at the same temperature for about 3 hours to obtain a reaction mixture of telmisartan methyl ester (I). Thereafter, the mixture is heated to about 55 C., and then 211 parts by weight of water is added dropwise in the range of 50 to 55 C. over about 1 hour to precipitate crystals, and then kept at the same temperature for 3 hours. The solution was cooled to 0 C., filtered, washed with methanol water, and dried at 50 C./1 kPa to obtain 42.8 parts by weight of telmisartan methyl ester (I) crystals. The crystals were analyzed by liquid chromatography.

The synthetic route of 152628-02-9 has been constantly updated, and we look forward to future research findings.

Application of 60-56-0, A common heterocyclic compound, 60-56-0, name is 1-Methyl-1H-imidazole-2(3H)-thione, molecular formula is C4H6N2S, 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.

General procedure: A vial charged with 1 (0.25 g, 0.753 mmol), KF/Al2O3 (0.7 g) thiol (1.1 mmol), and 18-crown-6 (0.05 g, 0.225 mmol) in 5 mL of acetonitrile was heated for 20 h at 80 C. Then solvent was evaporated under reduced pressure and crude product was purified by flash chromatography on silica gel using the mixture petroleum ether – ethylacetate as eluent.

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.

Electric Literature of 104619-51-4,Some common heterocyclic compound, 104619-51-4, name is Di(1H-imidazol-1-yl)methanimine, molecular formula is C7H7N5, 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.

An oven-dried, round-bottomed flask was chargedwith di(lH-imidazoI-I-yl)methanimine (1.40 g, 8.69 mmol),2-amino-5-methylphenol (713 mg, 5.79 mmol) and anhydrous THF (20 ml) at ambient temperature. The resulting suspension was refluxed underN2 (g) for 2 h. The solvent wasremoved in vacuo and the residue was purified by silica gelchromatography (0-30% 9: I methanol:annnonium hydroxide-chloroform) to afford benzo[d]oxazol-2-amine (792 mg,5.35 mmol, 92% yield), as a grey solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Di(1H-imidazol-1-yl)methanimine, its application will become more common.

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 95470-42-1 as follows. Quality Control of Ethyl 2-bromo-4-methyl-1H-imidazole-5-carboxylate

A solution of 2-bromo-4-methyl-lH-imidazole-5- carboxylic acid ethyl ester (1.0 g, 4.29 mmol) in dimethylformamide (DMF, 30 ml) was cooled to O0C, added with 60percent sodium hydride (NaH, 343 mg, 8.58 mmol) and stirred for 30 min. Iodomethane (0.8 ml, 12.87 mmol) was slowly added in droplets to the resulting solution which was then heated from 00C to room temperature with stirring for 4 hrs and added with water, followed by extraction with ethyl acetate. The extract was dried over MgSO4, filtered and concentrated in a vacuum. The purification of the concentrate thus obtain through silica gel column chromatography(hexane : ethyl acetate=5:l) afforded the object compound as a white solid (693 mg, 2.81 mmol, 65percent) . 1H-NMROOO MHz, CDCl3) sigma 1.38 (t, 3H, J = 7.1 Hz) ,2.46(s, 3H) , 3.88(s, 3H) , 4.33(q, 2H, J = 7.1 Hz); MS 246 (M+) .

According to the analysis of related databases, 95470-42-1, the application of this compound in the production field has become more and more popular.

Application of 17325-26-7, 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. 17325-26-7, name is Methyl 1H-imidazole-5-carboxylate belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

1H-Imidazole-4-carboxylic acid methyl ester (1.8 g, 14 mmol, Aldrich) reacted with bromine (1.6 mL, 29.8 mmol, Adrich) in acetic acid (20 mL) was stirred at RT for 12 h. The reaction mixture was filtered from the yellow precipitate, and the filter cake was washed with DCM (2*20 mL). The cake was mixed with sat. aqueous solution of NaHCO3 (100 mL) and EtOAc (200 mL), and the mixture was stirred for 1 h at RT. The organic layer was separated and the aqueous phase was extracted with EtOAc (2*200 mL). The organic extracts were combined, dried over MgSO4 and filtered. The filtrate was concentrated and the residue was purified by preparative HPLC [gradient 10-85% MeCN (0.1% TFA)/H2O (0.1% TFA)] to give the title compound as light-yellow solid. MS (ESI, positive ion) m/z: 282, 284 (M+I).

The synthetic route of Methyl 1H-imidazole-5-carboxylate has been constantly updated, and we look forward to future research findings.

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. 68282-47-3, name is 2-Phenyl-1H-imidazole-4-carbaldehyde, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C10H8N2O

a 4-Aminomethyl-2-phenylimidazole dihydrochloride Hydroxylamine hydrochloride (229 mg, 3.3 mmol) was added to a suspension of 2-phenylimidazole4-carboxaldehyde (516 mg, 3 mmol; prepared according to J. Chem. Soc. Perkin Trans. I 1974, 1527) and sodium acetate (541 mg, 6.6 mmol) in absolute EtOH (5 mL) and H2 O (5 mL) at RT. A yellow, homogeneous solution was produced. After 15 min, the reaction was concentrated on the rotavap to remove the EtOH, and the oily, aqueous mixture was extracted with 20% MeOH/CHCl3 (10 mL) then with CHCl3 (10 mL). The combined organic layers were dried (MgSO4) and concentrated to leave a yellow foam. The yellow foam was dissolved in absolute EtOH (9 mL), and 1.0 N HCl (6 mL, 6 mmol) and 10% Pd/C (0.32 g, 0.3 mmol) were added. The mixture was shaken on a Parr apparatus at RT under H2 (50 psi) for 4 h, then was filtered through Celite. The filtrate was concentrated on the rotavap to leave a light yellow solid. Recrystallization fron absolute EtOH/H2 O gave the title compound as a light pink solid (465 mg, 63%): mp 273-275 C. (dec.); 1 H NMR (250 MHz, CD3 OD) delta 7.93-8.12 (m, 2H), 7.80 (s, 1H), 7.50-7.76 (m, 3H), 4.40 (s, 2H); MS (ES) m/e 347.2 (2M+H)+, 174.0 (M+H)+, 157.0 (M+H–NH3)+.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 68282-47-3.