Tag: M.W=100-200

Application of 4856-97-7, 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 4856-97-7 as follows.

Into a 100 ml three neck RB flask containing Ar(g) was placed DMF (40 ml), followed by (lH-benzo[d]imidazol-2-yl)methanol (2.20 g, 14.9 mmol), thus forming a pale orange solution. This was cooled to 0 °C and 60percent sodium hydride (0.772 g, 19.3 mmol) was added in one portion. After stirring for 10 min under Ar(g) at 0 °C, 4-bromobutanenitrile (2.64 g, 17.8 mmol) was added in one portion. The reaction was allowed to warm to rt and left to proceed for 18 h. The reaction mixture was diluted with DCM and then poured onto a brine solution. The organic layer was separated and the aqueous phase was extracted three times with DCM. The combined organic fractions were dried over anhydrous sodium sulfate and then concentrated in vacuo. Purification by column chromatography (100percent DCM to 3percent MeOH/DCM) afforded the desired product as a viscous oil which solidified to a white solid over a period of hours (2.99 g, 13.9 mmol, 94percent). 1H NMR (400 MHz, DMSO-d6) delta 7.60-7.53 (m, 2H), 7.26 – 7.19 (m, 1H), 7.19 – 7.13 (m, 1H), 5.65 (t, J = 5.8 Hz, 1H), 4.70 (d, J = 5.8 Hz, 2H), 4.39 – 4.25 (m, 2H), 2.56 (t, J = 7.3 Hz, 2H), 2.15 – 2.01 (m, 2H)

According to the analysis of related databases, 4856-97-7, the application of this compound in the production field has become more and more popular.

Application of 13435-22-8, 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. 13435-22-8, name is 1-Butyl-2-methyl-1H-imidazole, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: 2.3. Typical procedure for the synthesis of imidazolium ion tethered TsDPENs 5a. A solution mixture of the intermediate 3 (818 mg, 1.5 mmol) and 1,2-dimethyl-1H-imidazole (173 mg, 1.8 mmol) in acetonitrile (2 mL) was heated at 70 C for 30 h. The solvent was removed under reduced pressure, and the residue was washed with a mixture solvent (hexane/ethyl acetate = 10:1) and dried in vacuo to give an intermediate 4a, to which HCl solution (3 mL, 4 M in dioxane) was added. The reaction mixture was stirred at room temperature for 5 h and the precipitation was filtered and washed with hexane to give the Boc deprotected intermediate, which was used for the next step directly without further characterization. The Boc-deprotected intermediate was subsequently neutralized by Na2CO3 (159 mg, 1.5 mmol) in MeOH (2 mL). The mixture was stirred for 5 h and the solvent was removed to dryness. The solid residue was dissolved in dry CH2Cl2 and filtered, and concentrated to give the product 5a as a white solid (550 mg, 68% yield for 2 steps).

The chemical industry reduces the impact on the environment during synthesis 1-Butyl-2-methyl-1H-imidazole. I believe this compound will play a more active role in future production and life.

Application of 137049-00-4,Some common heterocyclic compound, 137049-00-4, name is 1-Methyl-1H-imidazole-4-sulfonyl chloride, molecular formula is C4H5ClN2O2S, 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.

3. Synthesis of (1-(1-Methyl-1H-Imidazol-4-ylsulfonyl)Piperidin-4-yl)(Phenyl)Methanone, 4; To a solution of 4-benzoylpiperidine hydrochloride (1.50 g, 6.64 mmol) and DIPEA (2.74 mL, 15.3 mmol) in CH2Cl2 (35 mL) was added 1-methylimidazole-4-sulfonyl chloride (1.31 g, 7.31 mmol) and stirred for 18 h. The reaction was washed with 2 N NaOH (30 mL), dried over MgSO4 and concentrated under vacuum to afford 4 as a white solid (2.05 g, 93%); 1H-nmr (400 MHz, CDCl3) delta 7.81-7.78 (m, 2H), 7.52-7.36 (m, 5H), 3.86-3.78 (m, 2H), 3.71 (s, 3H), 3.26-3.17 (m, 1H), 2.82 (td, J=11.0, 3.0 Hz, 2H), 1.92-1.84 (m, 4H); m/z 334.0 [M+H].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-1H-imidazole-4-sulfonyl chloride, its application will become more common.

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. 6775-40-2, name is 5-Phenyl-1H-imidazol-2-amine belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C9H9N3

General procedure: To a stirred solution ofaldehyde (1 mmol), amine (1 mmol), CCl3CN (2 mmol) in PEG-400 (5mL) at 0 oC, a solution of H2O2 (30%) (3mmol)was added drop wise. Then the reaction mixture was stirred at room temperature for 8-12 h. After completion ofthe reaction (monitored by TLC), the reaction mixture was poured into ice water (50 mL). The solid obtained wasfiltered, washed with water and crude product was purified by column chromatography (silica gel, 60-120 mesh)using hexane/ethylacetate (6:4) as eluent.

The synthetic route of 6775-40-2 has been constantly updated, and we look forward to future research findings.

Related Products of 312-73-2, 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. 312-73-2 name is 2-(Trifluoromethyl)-1H-benzo[d]imidazole, 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 solution of 2-(trifluoromethyl)-1H-benzo[d]imidazole (2 g, 10.7 mmol) in H2SO4 (55.2 g, 30 mL, 535 mmol) was added slowly hydrogen peroxide (35% solution, 10.4 g, 9.41 mL, 107 mmol) at 0-5 C. The reaction mixture was stirred at 120 C. for 3 h, cooled to RT, poured into water (80 mL) under ice bath cooling and extracted with diethyl ether (3*80 mL). The combined organic phase was dried over MgSO4, filtered and evaporated to give the product as colorless solid (1.98 g, 8.84 mmol, 82.2%) which was used without further purification for the next step. MS: M=225.4 (M+H)+

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(Trifluoromethyl)-1H-benzo[d]imidazole, and friends who are interested can also refer to it.

16265-04-6, name is 2-Chloro-1H-imidazole, belongs to imidazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 16265-04-6

4 g of 98% sulfuric acid, 2.04 g of 2-chloroimidazole ((? 02 mol) was added to the three-necked flask, and the mixture was stirred at room temperature (? 5h,And then heated to 45 ~ 55 C, slowly dropping from 1. 9g95% fuming nitric acid (0. 03mol) and 5g 20% fuming sulfuric acid composition of the mixed acid, after dropping, the temperature to 110 C reaction lh, the end After the reaction solution was poured into ice water, the pH was adjusted to 3 to 4 with aqueous ammonia, filtered and the cake was dried to give a white powdery solid 2-chloro-4-nitroimidazole, 56 mg, yield 87.3% HPLC purity 99. 4%, melting point 218. 6 ~ 219.5 C.

The synthetic route of 16265-04-6 has been constantly updated, and we look forward to future research findings.

Application of 4857-06-1, These common heterocyclic compound, 4857-06-1, name is 2-Chloro-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.

General procedure: In a round bottom flask fitted with amagnetic stirrer, 2-chloro-1H-benzimidazole, 3, (0.50 g, 3.3 mmol) was dissolved in DMSO (3mL) and then NaH (60%; 0.19 g, 4.9 mmol) was added at 0 C and stirred for 1h. Next, benzylbromide (0.67 g, 3.9 mmol) was added to the suspension and the reaction was stirred at rt for 12h. Ice-cold water (15 mL) was added to the mixture and resulting precipitate was collected viafiltration. The filtrate was washed with water and dried under vacuum to give desired product, 4,as a white solid (0.75 g, 88%). LCMS: RT = 2.69 min., >98% 215 and 254 nm, m/z = 243.0 [M+ H]+. 1H NMR (499 MHz, CDCl3) delta 7.68 (d, J = 7.4 Hz, 1H), 7.35 – 7.24 (m, 5H), 7.16 (d, J =6.8 Hz, 2H), 5.38 (s, 2H). 13C NMR (126 MHz, CDCl3) delta 141.33, 134.83, 128.99, 128.22, 126.76,123.53, 123.05, 119.18, 109.98, 47.94.

Statistics shows that 2-Chloro-1H-benzo[d]imidazole is playing an increasingly important role. we look forward to future research findings about 4857-06-1.

Adding a certain compound to certain chemical reactions, such as: 17325-26-7, name is Methyl 1H-imidazole-5-carboxylate, 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 17325-26-7, Product Details of 17325-26-7

EXAMPLE 1 12-{2-[4-chloro-3-(methyloxy)phenyl]-1 H-imidazol-4-yl}-N,N-dimethyl-1-[2-(m1 H-benzimidazole-5-carboxamidestep 1 s epstep 6Step 1. methyl 1 -({[2-(trimethylsilyl)ethyl]oxy}methyl)-1 /-/-imidazole-4-carboxylate: A mixture of methyl 1 H-imidazole-4-carboxylate (2.80 g, 22.20 mmol), {2-[(chloromethyl) oxy]ethyl}(trimethyl)silane (5.1 1 mL, 28.9 mmol) and potassium carbonate (7.67 g, 55.5 mmol) in DMF (20 mL) was heated at 80C for 24 hours. Reaction showed -1 :1 starting materiahdesired product by TLC. The reaction was cooled to room temperature, diluted with ethyl acetate and water, and layers were separated. Organics were washed with brine, concentrated and purified by Biotage (50 g silica column, 10-75% E/H, 20 min.; 75%, 10 min.). Clean fractions were combined, concentrated and dried to give the title compound as a light yellow oil (2.46 g, 45%). 1H NMR (400 MHz, DMSO-d6) delta 8.02 (d, J 1.26 Hz, 1 H), 7.92 (d, J = 1 .26 Hz, 1 H), 5.37 (s, 2H), 3.74 (s, 3H), 3.44 – 3.52 (m, 2H), 0.80 – 0.88 (m, 2H), -0.03 (s, 9H); MS (m/z) 257.0 (M+H)+.

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.

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. 1457-58-5, name is 2-Methyl-1H-imidazole-5-carboxylic acid belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C5H6N2O2

a) (S)-N-(l -(3 -(3 -chloro-4-cyanophenyl)- 1 H-pyrazol- 1 -yl)propan-2-yl)-2- methyl- 1 H-imidazole-4-carboxamide2-Methyl-lH-imidazole-4-carboxylic acid (29.0 g, 230 mmol), 335 ml of DMF and 165 ml of DCM were placed in to the reaction vessel under nitrogen.HBTU (7.27 g, 19.18 mmol), EDCI (44.1 g, 230 mmol) and 66.8 ml of DIPEA were added. (S)-4-(l-(2-aminopropyl)-lH-pyrazol-3-yl)-2-chlorobenzonitrile (50 g, 192 mmol) was added and the reaction stirred overnight at RT. 600 ml of water was slowly added and water phase was washed with 335 ml and 500 ml of DCM. DCM phases were combined, washed with 3 x 600 ml of water and distilled to dryness. Acetonitrile (300 ml) was added and the mixture was heated up to 75C. Water (300 ml) was added at >60 C, solution was allowed to cool to RT for precipitation and the mixture was stirred overnight at RT. Stirring was continued for additional 2 h at <10 C. The precipitate was filtered, washed with cold ACN: water and dried under vacuum to obtain 47 g of crude product. The title compound was recrystallized from EtOH with 75 % yield. -NMR (400 MHz, DMSO-

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 3314-30-5 as follows. Quality Control of 1H-Benzo[d]imidazole-2-carbaldehyde

General procedure: A suspension of methyl 2-(2-aminoethyl)-1 ,3-thiazole-4-carboxylate (5) (1.96 g, 10.52 mmol), 1 H- benzimidazole-2-carbaldehyde (2.31 g, 15.79 mmol) and DIPEA (1.83 ml, 10.52 mmol) in MeOH (100 ml) was stirred at room temperature for 12 h. The reaction mixture was cooled to 0°C, NaBH4 (0.597 g, 15.79 mmol) was added and the mixture stirred at room temperature for 2 h. The reaction mixture was concentrated in vacuo and the residue dissolved in EtOAc (100 ml) and washed with saturated NC03 (2 x 50 ml). The combined aqueous layers were extracted with EtOAc (3 x 50 ml) and the combined organic layers dried (MgS04), filtered and evaporated in vacuo. Purification by flash column chromatography (KP- NH, eluting with a gradient of 0-10percent MeOH / DCM) afforded the title compound (1.4 g, 38percent, 90percent purity) as a tan solid. 1 H-NMR (Methanol-d4, 250 MHz): d[ppm]= 8.27 (s, 1 H), 7.60 – 7.49 (m, 2H), 7.29 – 7.17 (m, 2H), 4.09 (s, 2H), 3.92 (s, 3H), 3.26 (t, J = 6.3 Hz, 2H), 3.10 (t, J = 6.8 Hz, 2H) HPLCMS (Method A): [m/z]: 317 [M+H]+In a similar fashion using general procedure 3, (3S)-1-(2-aminoethyl)-N-[(3-fluoropyridin-2- yl)methyl]pyrrolidine-3-carboxamide (438) (150 mg, 0.56 mmol), 1H-1,3-benzodiazole-2-carbaldehyde (82 mg, 0.56 mmol) and DIPEA (196 muIota, 1.13 mmol) in MeCN (10 ml) at room temperature for 16 h, followed by the addition NaBH4 (31 mg, 0.81 mmol) gave the title compound (47 mg, 21percent) as a pale yellow film after purification by basic prep-HPLC. 1H-NMR (MeOD, 500 MHz): d[ppm]= 8.31 – 8.26 (m, 1 H), 7.54 – 7.48 (m, 3H), 7.32 – 7.27 (m, 1 H), 7.23 – 7.17 (m, 2H), 4.55 (d, J= 1.5 Hz, 2H), 4.03 (s, 2H), 3.05-2.97 (m, 1H), 2.83-2.76 (m, 3H), 2.75-2.60 (m, 5H), 2.15-2.06 (m, 1H), 2.06- 1.97 (m, 1H) HPLCMS (Method C): [m/z]: 397.2 [M+H]+

According to the analysis of related databases, 3314-30-5, the application of this compound in the production field has become more and more popular.