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. 872-49-1, name is 5-Chloro-1-methylimidazole, A new synthetic method of this compound is introduced below., Application In Synthesis of 5-Chloro-1-methylimidazole

An acetonitrile (6 ml) solution of 2,5-difluorobenzaldehyde (327 mul, 3 mmol), 5-chloro-1-methylimidazole (187 mug, 2 mmol) and di-t-butyl dicarbonate (504 mul, 2.2 mmol) was stirred at room temperature for 20 hours. The precipitate thus formed was collected by filtration, followed by trituration with hexane to give the title compound (472 mg, 66%) as a white solid. 1H-NMR (400MHz, CDCl3) delta: 1.48(9H,s), 3.67(3H,s), 6.88-7.1 (4H, m), 7.39 (1H, m). mp: 125 to 126C. MSm/z: 359 (M++H) .

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 17325-26-7, 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. 17325-26-7, name is Methyl 1H-imidazole-5-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

lambda/-bromosuccinimide (0.900 g, 5.0 mmol) was added to a stirred solution of methyl 1 H-imidazole-4-carboxylate (0.630 g, 5.0 mmol) in CH3CN (50 mL). The reaction mixture was stirred for 12 h in the dark and then concentrated in the presence of silica gel. The absorbed crude material was purified by column chromatography (20- 100% EtOAc/hexanes) to afford the title compound (0.708 g, 70%) as a white solid. 1H NMR (400 MHz, DMSOd6) delta ppm 1 1.00 (br. s., 1 H), 7.81 (s, 1 H), 3.81 (s, 3 H). ES-LCMS: m/z 204.9, 206.9 (M+1 ).

The chemical industry reduces the impact on the environment during synthesis Methyl 1H-imidazole-5-carboxylate. I believe this compound will play a more active role in future production and life.

Related Products of 53484-15-4,Some common heterocyclic compound, 53484-15-4, name is 5-Bromo-1-methyl-1H-benzo[d]Imidazole, molecular formula is C8H7BrN2, 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.

[000388j To a stirred solution of compound 1 (1.6 g, 1 eq) in aq. ammonia solution (5 mL), copper chloride (catalytic amount) was added and heated at 90 C in a sealed tube for 18 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was evaporated to dryness. The residue was stirred with 20% methanol in dichloromethane and filtered. The filtrate was evaporated under reduced pressure to afford the title compound 2. LCMS (mlz): 148.00 (M + 1).

The synthetic route of 53484-15-4 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 583-39-1, These common heterocyclic compound, 583-39-1, name is 2-Mercaptobenzimidazole, 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 method: Benzimidazole-2-thiol (7) (1 eq) and pertinent acid chloride or acid anhydride (1.1 eq) were dissolved in pyridine (4.4 eq) under a nitrogen atmosphere. The reaction mixture was stirred overnight at room temperature. After quenching with water (10-25 ml), ethyl acetate (30-45 ml) was added. The organic phase was extracted with 3M hydrochloric acid (3 × 25 ml), dried over magnesium sulfate and concentrated under reduced pressure. The crude product was purified as stated below.

The synthetic route of 583-39-1 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 934-22-5, 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. 934-22-5, name is 6-Aminobenzimidazole belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A solution of 1 H-benzo[d]imidazol-5-amine (1 eq.) and the respective aldehyde (1 eq.) in dry methanol (3 ml in case of 1 mmol) was stirred at room temperature for 3 hours. After addition of 2-(ethoxycarbonyl)acetic acid (1 eq.) and 1-isocyano-2-methylpropan-2-yl methyl carbonate (1 eq.) stirring was continued for 16 hours. The solvent was evaporated and the residue was purified by flash chromatography on silica gel using a CHCl3/MeOH gradient.

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, 6-Aminobenzimidazole, other downstream synthetic routes, hurry up and to see.

Some common heterocyclic compound, 1546-79-8, name is 2,2,2-Trifluoro-1-(1H-imidazol-1-yl)ethanone, molecular formula is C5H3F3N2O, 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: 1546-79-8

To a solution of 5 (1.54 g, 2.67 mmol) in THF (40 mL) was added 1-(trifluoroacetyl)imidazole (365 mL, 3.20 mmol), and the whole was heated for6 h under reflux. After being cooled to room temperature, the reactionmixture was quenched by addition of ice, and the solvent was removedin vacuo. The residue was partitioned between AcOEt and H2O. The separatedorganic layer was further washed with H2O (twice) and saturatedaqueous NaHCO3, followed by brine. The separated organic layer wasdried and concentrated in vacuo. The residue was purified by a silica gelcolumn, eluted with MeOH in CHCl3 (0%-4%), to give 6 (1.30 g, 84% asa white solid): ESI-LRMS m/z 601 (MNa); ESI-HRMS calcd forC29H54N4O4NaSi2 601.3581, found 601.3539; 1H NMR (400 MHz, CDCl3)d 7.73 (1 H, s, H-2), 7.01 (1 H, br s, NH2, exchangeable with D2O), 6.09(1 H, dd, H-1?, J5.4, 8.3 Hz), 5.39 (1 H, br s, NH2, exchangeable withD2O), 4.88 (1 H, d, CH2, J18.0 Hz), 4.72 (1 H, dd, H-3?, J2.3, 5.3 Hz),4.13-4.08 (2 H, m, H-4?,CH2), 3.90-3.83 (2 H, m, H-5?), 2.55 (1 H, ddd,H-2?a, J5.4, 13.0, 2.3 Hz), 2.44 (1 H, ddd, H-2?b, J8.3, 13.0, 5.3 Hz),1.16-1.02 (42 H, m, TIPS); 13C NMR (100 MHz, CDCl3) d 165.08, 134.74,132.94, 124.22, 115.69, 89.14, 85.36, 72.78, 63.57, 42.63, 18.09, 18.06,13.14, 12.18, 11.99.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1546-79-8, its application will become more common.

Electric Literature of 116568-17-3, 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 116568-17-3 as follows.

Example 18; 4-Benzylpiperidine-l-carboxylic acid (lH-benzoimidazol-5-carbonyl)-amide [the other tautomeric form of the compound is 4-benzyIpiperidin-l-carboxylic acid (3H-benzoimidazol-5-carbonyl)-amide1; To a Suspension of 0.947 g (3.08 mmol) of lH-benzoimidazol-5-carboxylic acid amide [Bull. Chem. Soc. Jpn., 31j 252 (1958)] in 50 ml of 1,2-dichloroethane 0.5 ml (5.7 mmol) of oxalyl chloride is added and the mixture is stirred at 90 C for 5.5 h. The reaction mixture is cooled to room temperature and 2.65 ml (15 mmol) of 4-benzylpip.eridine is added. The so obtained mixture is stirred at room temperature overnight, then concentrated and the residue is purified by column chromatography using Kieselgel 60 aes adsorbent (Merck) and Chloroform : methanol = 9 : l aes eluent to yield 145 mg (13 %) of the title compound. Mp.: 168-175 C .

According to the analysis of related databases, 116568-17-3, 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. 39070-14-9, name is (1-Methyl-2-nitro-1H-imidazol-5-yl)methanol, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: (1-Methyl-2-nitro-1H-imidazol-5-yl)methanol

Step 2: To a solution of compound G2 (3.41mmol) in THF cooled to -12C was added dropwise phosphorus oxychloride (5.12 mmol). The reaction mixture was stirred at -12C for 40minutes and then, proton sponge (13.64mmol) was added. The reaction mixture was stirred at -12C overnight. To this stirred reaction mixture was added a solution of benzylamine (3.75mmol) and triethylamine (17.05mmol) in acetonitrile (7mL).The reaction mixture was then allowed to warm to -5C. The reaction mixture was stirred for 5 hours. The reaction was monitored by LC/MS. To the reaction mixture was then added a solution of (3-methyl-2-nitro-3H-imidazol-4-yl)-methanol (10.23mmol) and 4-(dimethylamino)pyridine (10.23 mmol) in acetonitrile (10 mL). The reaction mixture was stirred at room temperature overnight, and then concentrated under reduced pressure. The crude residue was partitioned between a 5% solution of citric acid and ethyl acetate. The organic layer was washed with water and brine, dried over over sodium sulfate, filtered and concentrated under reduced pressure. The crude residue was purified by flash chromatography on silica gel (DCM/methanol: 0 to 3%) to afford the expected compound G3.

According to the analysis of related databases, 39070-14-9, the application of this compound in the production field has become more and more popular.

Application of 4887-80-3, These common heterocyclic compound, 4887-80-3, name is 5-Methoxy-1H-benzo[d]imidazole, 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.

Example 92; 4-(lH-Benzoimidazol-5-yloxy)-N-(4-bromo-phenyl)-3-(7-isopropyl-pyrido[2,3-d]pyrimidin-4- ylamino)-benzamide; Example 92A; lH-Benzoimidazol-5-ol; [0458] A solution of 5-methoxybenzimidazole (500 mg, 3.374 mmol) in 48% hydrobromic acid (10 mL) was refluxed for 2 hours. The reaction was cooled to room temperature, the solvent removed by rotary evaporation under vacuum, and the residue azeotroped with toluene (50 mL) to provide the title compound as a tan solid (701 mg, 96%).

The synthetic route of 4887-80-3 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 616-47-7, name is 1-Methyl-1H-imidazole, 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 616-47-7, name: 1-Methyl-1H-imidazole

(Comparative Examples 1 to 4) 1-methyl-1H-imidazole 3.3 g scaleAfter replacing the inside of a 100 mL three-necked flask with an argon atmosphere, 22 mL of acetonitrile, 3.3 g of 1-methyl-1H-imidazole and triethylamine in the amounts shown in Table 1 were added and cooled to -20 C. To this solution, a solution of ethyl chloroformate in the amount shown in Table 1 in 8 mL of acetonitrile was added at the addition time shown in Table 1. Thereafter, the mixture was stirred at room temperature for the reaction time shown in Table 1. To the reaction solution were added 20 mL of ethanol and 10 mL of water to dissolve the precipitate, and 1 mL was collected from the homogenized solution. The collected solution was diluted 1000-fold with acetonitrile and subjected to HPLC analysis, and the yield was calculated. The results are shown in Table 2.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-imidazole, and friends who are interested can also refer to it.