Month: April 2021

Related Products of 20485-43-2,Some common heterocyclic compound, 20485-43-2, name is 1-Methyl-1H-imidazole-2-carboxylic acid, molecular formula is C5H6N2O2, 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: Reaction monitoring. To check the progress of the reaction, some resin beadswere taken, mixed with 30 muL of 95% TFA solution and shaken for a fewseconds, while the beads turn red. The supernatant solution was removed andmixed 1:1 with H2O. 1 muL of the aqueous solution was mixed with 1 muL of DHBmatrix on the target, dried and the mass spectrum was measured by MALDI-ToF-MS. If necessary, the deprotection was repeated.Fmoc deprotection. The amino protecting group Fmoc was cleaved after eachcoupling step to allow the coupling of the next amino acid. For this, the resinwas swollen in DMF and then suspended three times for 15 minutes in a 20%piperidine solution in DMF. The resin was filtered off and washed twice withCH2Cl2, DMF and again CH2Cl2.Coupling reactions. The resin was swollen in DMF. The amino acid (3 equiv)was dissolved in DMF containing DIPEA (9 equiv) and the coupling reagent(HBTU or PyBOP, 3 equiv) was added for pre-activation. After 5 minutes thesolution was added to the resin, and the suspension was mixed for 1.5 hours byshaking. The resin was then filtered off with suction and washed twice withCH2Cl2, DMF and again CH2Cl2. The completeness of the reaction was checkedwith MALDI-ToF-MS. If necessary, the coupling reaction was repeated.Cleavage from the resin. After swelling in CH2Cl2, the acid-labile 2 chlorotritylresin containing the polyamide was mixed with a 2.5% solution ofS7CH2Cl2/TFA/TIS 95:2.5:2.5 (v/v/v), mixed for 5 minutes and filtered off. This wasrepeated until the discoloration of the filtrate was complete. The combinedfiltrates were evaporated and the oily residue was treated with a mixtureH2O:MeCN and lyophilized.

The synthetic route of 20485-43-2 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 1402838-08-7, name is 2-(1-Trityl-4-imidazolyl)benzaldehyde, 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. Application In Synthesis of 2-(1-Trityl-4-imidazolyl)benzaldehyde

To a three-necked flask was added 2- (1-trityl-1H-imidazole-4-) benzaldehyde (400 mg, 0.97 mmol)Acetyl-1-deuterated cyclohexane (122 mg, 0.97 mmol)And anhydrous tetrahydrofuran (5 ml)Under nitrogen protection,A solution of sodium ethoxide (85 mg, 1.25 mmol) in ethanol was added at room temperature,Stir at room temperature for 3 h, spin dry solvent,Saturated ammonium chloride (10 ml) was added, Extracted with ethyl acetate, the combined organic layers were dried over anhydrous sodium sulfate, the solvent was dried,Acetic acid (1 ml) and ethanol (5 ml) were added,Was stirred at 90 3h, cooled to room temperature,The organic layer was combined and dried over anhydrous sodium sulfate. The solvent was concentrated and purified by column chromatography on silica gel to give compound 23 (210 mg, yield: 77%), and the residue was extracted with ethyl acetate.

The synthetic route of 2-(1-Trityl-4-imidazolyl)benzaldehyde has been constantly updated, and we look forward to future research findings.

Application of 14741-71-0,Some common heterocyclic compound, 14741-71-0, name is Ethyl 2-(1H-benzo[d]imidazol-2-yl)acetate, molecular formula is C11H12N2O2, 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.

Step 3: 4-Amino-3-(1H-benzimidazol-2-yl)-5-(4-ethylpiperazin-1-yl)quinolin-2(1H)-one t-BuLi (3.1 equivalents) was added to ethyl 2-benzimidazol-2-ylacetate (1.0 equivalent) and 6-amino-2-(4-ethylpiperazinyl) benzenecarbonitrile (1.0 equivalent) in THF at 0 C. The reaction was stirred overnight. The resulting mixture was quenched with NH4Cl (aqueous saturated) and extracted with EtOAc. The combined organic layers were washed with H2O and brine, dried over Na2SO4, filtered, and concentrated in vacuo to yield a brown solid. The crude material was triturated with CH2Cl2 and MeOH to provide a tan solid. LC/MS m/z 389.1 (MH+), Rt 1.80 minutes.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 2-(1H-benzo[d]imidazol-2-yl)acetate, its application will become more common.

Electric Literature of 3034-50-2, 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. 3034-50-2, name is Imidazole-4-carbaldehyde, This compound has unique chemical properties. The synthetic route is as follows.

To a mixture of acetophenone 7 (0.56g, 3.0mmol) and imidazole-4-carbaldehyde (0.29g, 3.0mmol) in ethanol (25mL) was added 10% sodium hydrate aqueous (5mL), the mixture was stirred for 24h at room temperature [17]. The solution was acidified with 1N HCl and filtered, and the filter cake was recrystallized from ethanol got 8 as white power (0.60g). Yield: 87.4%; mp: 185-186C; IR (KBr, cm-1) nu: 3443 (OH), 3063 (Ar-H), 1719 (C=O), 1617, 1571 (aromatic frame); 1H NMR (400MHz, DMSO-d6) delta: 11.44 (s, 1H, OH), 7.91 (s, 1H, imidazole-2-H), 7.79 (s, 1H, imidazole-5-H), 7.59 (d, J=8.4Hz, 1H, flavone-5-H), 6.85 (d, J=1.8Hz, 1H, flavone-3-H), 6.77-6.72 (m, 2H, flavone-6-H, flavone-8-H) ppm; 13C NMR (101MHz, DMSO-d6) delta: 181.2, 167.7, 166.9, 146.0, 138.0, 130.6, 126.0, 113.9, 113.3, 104.1, 99.0ppm; MS (m/z): 229 [M+H]+; HRMS (TOF) calcd for C12H8N2O3: [M+H]+, 229.0613; found, 229.0617.

The chemical industry reduces the impact on the environment during synthesis Imidazole-4-carbaldehyde. I believe this compound will play a more active role in future production and life.

Electric Literature of 30148-21-1, 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. 30148-21-1, name is Ethyl 1-methyl-1H-imidazole-2-carboxylate belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

(S)-[2-(hydroxydim-tolylmethyl)pyrrolidin-1-yl](1-methyl-imidazol-2-yl)methanone was first prepared by dissolving (S)-a,a-Di(3-methylphenyl)prolinol (prepared as described above, 0.8 g, 2.85 mmol) in toluene (10 mL) and NaH (60 % dispersion in mineral oil, 148 mg,3.7 mmol) added at room temperature. After stirring for 30 mins, ethyl-1-methylimidazole-2-carboxylate (527 mg, 3.4 mmol) was added. The resulting reaction mixture was slowly warm to 70 C and stirred for 24 h at the same temperature. The reaction was cooled to room temperature, quenched by addition of saturated aqueous NH4CI (20 mL) and extracted with dichloromethane (3 x 20 mL). The combined organic extracts were washed with brine (20 mL) and dried over magnesium sulfate. After filtration, the filtrate was evaporated and purified by chromatography on silica gel (10% to 50% ethyl acetate in petroleum ether) to yield the product (0.53 g, 48 %) as white solid; m.p. 162-164C;[a]D-95.5 (c1 .1 in CHCI3);vmax (thin film, cm -1) 2952, 1615, 1456, 1282; deltaEta (500 MHz, d6-DMSO, 100 C) 1 .66-1 .75 (m, 1 H, 1 xCH2), 1 .78-1 .86 (m, 1 H, 1 chi CH2), 1 .93-1 .97 (m, 1 H, 1 chi CH2), 2.05-2.12 (m, 1 H, 1 chi CH2), 2.14 (s, 3H, CH3), 2.29(s, 3H, CH3), 3.36 (s, 3H, NCH3), 3.47-3.52 (m, 1 H, 1 chi CH2), 3.87- 3.92 (m, 1 H, 1 x CH2), 5.68 (s, 1 H, NCH), 6.14 (br, s, 1 H, OH), 6.85-6.87 (m, 2H, ArH), 6.91 – 6.98 (m, 4H, ArH), 7.04 (app. d, 1 H, J 7.7, ArH), 7.18-7.24 (m, 2H, ArH), 7.28 (s, 1 H, ArH); deltaC (126 MHz, d6-DMSO, 100C) 20.6(2 x CH3), 22.2(CH2),27.2 (CH2), 33.6 (CH3),47.4(NCH2), 63.5(NCH), 80.1 (COH), 123.2, 123.3, 123.6, 125.3, 125.9, 126.2, 126.6, 126.9, 127.2, 135.2, 136.1 , 140.2, 145.3, 145.4, 158.9 ( CO) ;mlz (TOF ES+) 390.2188 (100%, MH+, C24H28N3O2 requires 390.2182), 372.2092 (20).

The synthetic route of Ethyl 1-methyl-1H-imidazole-2-carboxylate has been constantly updated, and we look forward to future research findings.

Related Products of 28890-99-5, 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. 28890-99-5 name is 5H-Benzo[d]benzo[4,5]imidazo[1,2-a]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.

c) 5.00 g (13.4 mmol) 2-bromo-8-iodo-dibenzofuran, the synthesis of which is described in EP1885818, 8.74 g (26.8 mmol) caesium carbonate, 255 mg (1.34 mmol) copper(I) iodide and 309 mg (2.68 mmol) L-proline are added to 2.78 g (13.4 mmol) 5H-benzimidazo[1,2-a]benzimidazole in 75 ml dimethylformamide under nitrogen. The reaction mixture is heated for 19 h at 150 C. and filtered on Hyflo Super Cel medium, Fluka 56678, CAS [91053-39-3] with THF. The organic phase is washed with water. The solvent is distilled off. Column chromatography on silica gel with toluene/ethyl acetate 19/1 results in compound 3 (yield: 2.29 g (37.7%)).1H NMR (400 MHz, THF-d8): delta 8.66 (s, 1H), 8.41 (s, 1H), 8-01-8-16 (m, 3H), 7.89 (d, J=8.8 Hz, 1H), 7.63-7.75 (m, 4H), 7.25-7.49 (m, 4H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5H-Benzo[d]benzo[4,5]imidazo[1,2-a]imidazole, and friends who are interested can also refer to it.

Electric Literature of 86604-86-6, 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. 86604-86-6, name is 2-Chloro-6-(trifluoromethyl)benzimidazole belongs to imidazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Example 2: 3-Phenyl-8-r5-(trifluoromethyl)-1 H-benzimidazol-2-yll-1-oxa-3,8-diazaspiro- [4.51decan-2-one; 2-Chloro-5-(trifluoromethyl)-1 H-benzimidazole (Intermediate 1 , 50 mg, 0.227 mmol), which is commercially available or can be prepared according to the procedure described herein, was dissolved in DMSO (1.5 ml). 3-Phenyl-1-oxa-3,8-diazaspiro[4.5]decan-2-one hydrobromide (for a preparation see US4244961 , 78.1 mg, 0.249 mmol) and DIPEA (0.1 19 ml) were added. The mixture was irradiated in a microwave twice at 150 0C for 30 min. The mixture was passed through a SPE-SCX cartridge eluting with DCM, MeOH and 2M ammonia in methanol in this order. The basic fractions were evaporated and the residue was purified by silica gel chromatography eluting with cyclohexane/EtOAc/MeOH: 1/1/0 to 9/9/2 to give the title compound (20.0 mg, 21.2%). 1 H-NMR (500 MHz, DMSO- d6): delta 11.86 (1 H, br s), 7.57 (2H, d), 7.45 (1 H, br s), 7.40 (2H, t), 7.34 (1 H, d), 7.26 (1 H, d), 7.14 (1 H, t), 3.93 (2H, s), 3.81-3.88 (2H, m), 3.55-3.65 (2H, m), 1.91-2.06 (4H, m); HPLC-MS, 2: 2.69 min, m/z 417 [M+H]+.

The synthetic route of 2-Chloro-6-(trifluoromethyl)benzimidazole has been constantly updated, and we look forward to future research findings.

Electric Literature of 4887-88-1, The chemical industry reduces the impact on the environment during synthesis 4887-88-1, name is 5-Bromo-1H-benzo[d]imidazole, I believe this compound will play a more active role in future production and life.

To a solution of (4,4-dimethylcyclohexyl)({3-[1-(triphenylmethyl)-1H-benzimidazol-6-yl]phenyl}methyl)amine and (4,4-dimethylcyclohexyl)({3-[1-(triphenylmethyl)-1H-benzimidazol-5-yl]phenyl}methyl)amine (0.18 g, 0.31 mmol) in tetrahydrofuran (3 mL) were added water (3 mL) and acetic acid (3 mL). The reaction mixture was heated at reflux for 1 h, then was allowed to cool to room temperature and was treated with 10% HCl (aq) until pH 2. The mixture was washed 2× EtOAc, then the aqueous phase was treated with solid K2CO3 until it reached pH 10, at which point it was extracted 3× CHCl3. The combined CHCl3 extracts were dried (Na2SO4) and concentrated in vacuo. The residue was taken up in Et2O and enough acetone to dissolve completely, then 4M HCl in dioxane was added until no more solid crashed out. The white solid was collected by filtration and dried under vacuum, providing the product {[3-(1H-benzimidazol-5-yl)phenyl]methyl}(4,4-dimethylcyclohexyl)amine hydrochloride (M+1) 334.2 ES, 1.30 min (LC/MS Method A).

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, 5-Bromo-1H-benzo[d]imidazole, other downstream synthetic routes, hurry up and to see.

Some common heterocyclic compound, 1072-84-0, name is 1H-Imidazole-4-carboxylic acid, molecular formula is C4H4N2O2, 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. SDS of cas: 1072-84-0

For synthesis of methyl imidazole-4-carboxylate (5), conc. H2SO4(1.5 mL) was added to a suspension of Im-CO2H (1.00 g, 8.92 mmol)in MeOH (20 mL), and themixture was refluxed for 24 h to give a solutionthat was then cooled to 0 C and neutralized to pH 8 using 5 MNaOH. Evaporation in vacuo left a white residue that was re-dissolvedin a minimal volume of boiling water; cooling the solution depositedwhite crystals of the ester that were collected, washed with cold H2O(1 × 5 mL), and dried in vacuo at r.t. for 24 h. Yield: 0.87 g (77%). 1HNMR (DMSO-d6): delta 7.74 (s, 1H, H5-Im), 7.65 (s, 1H, H2-Im), 2.51 (s,3H, CH3-Im). IR: 3105 (N-H, s), 2976, 2846 (C-H, m), 1619 (C=O,m), 1363 (s), 1156 (m), 864 (m). ESI-MS: 127 (M+). Anal. Calcd. forC5H6N2O2: C, 47.62; H, 4.80; N, 22.21. Found: C, 47.5; H, 4.85; N, 21.7.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1072-84-0, its application will become more common.

621-72-7, name is 2-Benzyl-1H-benzo[d]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. Quality Control of 2-Benzyl-1H-benzo[d]imidazole

Under an oxygen atmosphere, 0.30 mmol of 2-benzylbenzimidazole (1 g) and 2 mL of dimethyl sulfoxide were sequentially added to the Schlenk reaction tube.The reaction was stirred under constant temperature in an IKA (constant temperature heating magnetic stirrer) for 48 h. After the reaction is completed, it is cooled to room temperature. Quenched with distilled water.It was then extracted with ethyl acetate (3 x 20 mL). The organic layers were combined and dried over anhydrous sodium sulfate. Pure target product by column chromatography 2g (52.6mg, 79%).

The synthetic route of 621-72-7 has been constantly updated, and we look forward to future research findings.