Day: April 8, 2021

Adding a certain compound to certain chemical reactions, such as: 5775-82-6, name is 4-Bromo-1,3-dimethyl-1H-pyrazole, belongs to pyrazoles-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 5775-82-6, category: pyrazoles-derivatives

0142-1 2,2′-Azobis(isobutyronitrile) (27 mg) was added to a solution of 4-bromo-1,3-dimethyl-1H-pyrazole (286 mg) and N-bromosuccinimide (320 mg) in chlorobenzene (6 mL), followed by stirring at 80 C. for 7 hours. The reaction mixture was cooled to room temperature, and ethyl acetate and a saturated sodium hydrogen carbonate aqueous solution were added thereto. The organic layer was collected by separation, washed with a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure, thereby obtaining 4-bromo-3-(bromomethyl)-1-methyl-1H-pyrazole (465 mg) as a white solid. MS m/z (M+H): 253.

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.

Synthetic Route of 92525-10-5, A common heterocyclic compound, 92525-10-5, name is 3-Iodo-1-methyl-1H-pyrazole, molecular formula is C4H5IN2, 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) To a solution of 4-((benzyloxy)methyl)pyrrolidin-2-one (836 mg), 3-iodo-1-methyl-1H-pyrazole (856 mg), copper(I) iodide (80 mg) and tripotassium phosphate (1.7 g) in cyclopentyl methyl ether (20 mL) was added N1,N2-dimethylethane-1,2-diamine (87 muL). The reaction mixture was stirred at 120 C. for 22 hr, and diluted with ethyl acetate, and saturated aqueous ammonium chloride solution was added thereto. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (1.1 g). MS (ESI+): [M+H]+286.3.

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.

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 14531-55-6 as follows. Safety of 3,5-Dimethyl-4-nitro-1H-pyrazole

To a solution of 3,5-dimethyl-4-nitro-1H-pyrazole (2.5 g, 17.7 mmol) and caesium carbonate (6.06 g, 18.6 mmol) in DMF (50 mL) was added 2-bromoethyl methyl ether (2.59 g, 1.75 mL, 18.6 mmol). The mixture was heated at 100 C for 3.5 h. After cooling to room temperature, the mixture was poured into water and extracted with ethyl acetate (3x 50 mL).The combined organic layers were washed with brine (50 mL), dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (EtOAc/heptanes = 1/4 v/v%) to afford 1- (2-methoxyethyl) -3,5 -dimethyl-4- nitro-pyrazole (2.66 g, 75.4%) as a white crystalline solid.

According to the analysis of related databases, 14531-55-6, the application of this compound in the production field has become more and more popular.

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. 1453-58-3, name is 3-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Formula: C4H6N2

Potassium /-butoxide (3.9 g, 0.33 mmol) was dissolved in DMSO (25 mL). To this solution was added 3 -methyl pyrazole (2.7 g, 0.33 mmol) and the reaction was heated at 50 C for 30 min. l-Bromo-4-chloro-2-fluorobenzene (4.6 g, 0.22 mmol) was then added and the reaction was stirred at 50 C for 16 h. The reaction was cooled to RT and extracted with water and EtOAc, washed with brine, and dried over Na2S04) filtered and concentrated in vacuo. Purification by normal phase silica gel column chromatography (EtO Ac/heptane) provided l-(2- bromo-5-chlorophenyl)-3-methyl-lH-pyrazole and l-(2-bromo-5-chloroplienyl)-5-methyl-lH- pyrazole as a 4: 1 mixture that was used in the next step directly,The mixture from Step 1 (8 g, 0.39 mmol) was dissolved in 160 mL of THF and cooled to 0 C. /-Propyl magnesium chloride (2.0 M in THF, 23 mL) was added dropwise and the reaction stirred for 45 min, then ethyl trifluoroacetate (6 mL) was added. The reaction was stirred for 30 min at 0 C, then 10% HC1 was added dropwise (40 mL). The reaction was extracted with water and EtOAc, washed with brine, and dried over Na2S04, filtered, and concentrated in vacuo. Purification by normal phase silica gel column chromatography (EtOAc/heptane) provided l -(4- chloiO-2-(3-methyi-lH-pyrazol-l-yl)phenyl)-2,2,2-trifluoroethanone as a white solid.

The synthetic route of 1453-58-3 has been constantly updated, and we look forward to future research findings.

Reference of 2075-45-8,Some common heterocyclic compound, 2075-45-8, name is 4-Bromo-1H-pyrazole, molecular formula is C3H3BrN2, 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 solution of 4-bromo-lH-pyrazole (21.6 g, 147 mmol) in dichloromethane (400 mL) from Step 1 was added HCl (4 N in dioxane) (2.204 mL, 8.82 mmol )And ethoxyethylene (12.72 g, 176 mmol). After stirring the mixture for 30 min at rt, the reaction was quenched with aqueous NaHCO3 (30 mL), stirred at rt for 1 h, and the two layers were separated. The organic layer was washed with water, dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford 28 g of crude product. The material was purified by flash chromatography using silica gel using a hexane / ethyl acetate mixture as a solvate. A portion of the main product containing the uv activity was combined and concentrated in vacuo to afford 13.2 g (41%) of the desired product as a clear oil

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

Application of 37687-24-4, These common heterocyclic compound, 37687-24-4, name is Diethyl 3,5-pyrazoledicarboxylate, 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.

Crude 2-chloro- 1 -(1 -(4-methoxybenzyl)- 1 H-pyrazol-4-yl)ethanone (7.1 g, 21 mmol) was dissolved in acetonitrile (100 mL). Diethyl 1H-pyrazole-3,5-dicarboxylate (4.6 g, 21 mmol) was added, followed by K2C03 (5.9 g, 43 mmol), and the reaction mixture was stirred at 45 C for 1 hour. The reaction mixture was cooled to ambient temperature, diluted with EtOAc, filtered and concentrated. The residue was purified over silica gel to afford diethyl 1 -(2- (1 -(4-methoxybenzyl)- 1 H-pyrazol-4-yl)-2-oxoethyl)- 1 H-pyrazole-3 ,5-dicarboxylate (8.7 g, 20 mmol, 92 % yield) as a white solid.

The synthetic route of 37687-24-4 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, belongs to pyrazoles-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 1192-21-8, Safety of 1-Methyl-1H-pyrazol-5-amine

Degas a mixture of 2-(2-chloropyrimidin-4-yl)-6,6-dimethyl-5-(2- morpholinoethyl)thieno[2,3-c]pyrrol-4-one (20.8 g, 52.9 mmol), 2-methylpyrazol-3-amine (5.7 g, 58.2 mmol), cesium carbonate (37.9 g, 116.5 mmol), 4,5- bis(diphenylphosphino)-9,9-dimethylxanthene (2.6 g, 4.5 mmol) and 1,4-dioxane (529 mL) with nitrogen for 10 minutes. Add tris(dibenzylideneacetone)dipalladium(0) (2.4 g, 2.6 mmol) and heat the mixture to 85 C for four hours. Cool the mixture to room temperature and filter the mixture through filter paper. Concentrate the filtrate under reduced pressure. Repeat the reaction starting with 8 g of 2-(2-chloropyrimidin-4-yl)-6,6- dimethyl-5-(2-morpholinoethyl)thieno[2,3-c]pyrrol-4-one and combine the two residues. Purify the residue by silica gel column chromatography (330 g) eluting with a gradient from 5-25% MeOH in (10% EtOAc in DCM). Pool the fractions and concentrate under reduced pressure. Re-purify the residue by silica gel column chromatography (330 g) eluting with a gradient from 5-25% MeOH in 10% EtOAc in DCM. Pool the fractions and concentrate under reduced pressure. Dissolve the residue in DCM (400 mL) and then add acetone (1 L). Slowly concentrate the mixture under reduced pressure to approximately 700 mL. Collect the solid by vacuum filtration to give the title compound 14.8 g (48%). MS (m/z): 454 (M+1).

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.

Application of 1280210-79-8, 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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

INTERMEDIATE 6; 2-(2-Hydroxy-2-methylpropyl -2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-5-ium trifluoroacetate saltTo a stirred solution of tert-butyl 2,6-dihydropyrrolo[3 ,4-c]pyrazole-5(4H)-carboxyIate(35 g, 167 mmol) in DMF (500 mL) at 0 C under N2 was added sodium hexamethyldisilazide in THF (351 mL, 351 mmol) and the mixture was stirred at 0 C for 30 min. Isobutylene oxide (74.3 mL, 836 mmol) was then slowly added. The solution was stirred at 0C for 0.5 h and then stirred at room temperature for 1 h. The solution was heated to 80C for 100 min in a microwave oven, cooled to room temperature and evapoarted under vacuum. The residue was purified by column chromatography on silica gel, eluting with a gradient of 0% to 6% CH2Cl2 MeOH (containing 1 % NH4OH) to give a mixture of two regioisomers. The mixture of tworegioisomers A and B was resolved by chromatography on a ChiralPak AD-H column eluting with 4-40% MeOH/C02 to give isomer A as the faster eluting isomer and isomer B as the slower eluting isomer. NMR (500 MHz, CD3OD) for isomer B: 67.42 (d, 1 H); 4.42 (s, 2H); 4. 1 (s, 2H); 4.07 (s, 2H); 1.51 (d, 9H); 1.16 (s, 6H). LC-MS: 226.27 (M+l-56).The desired isomer B was treated with 1 :1 TFA/C?C12 for 1 h to give the title compound. NMR (500 MHz, CD3OD): 57.55 (s, 1H); 4.43 (s, 2H); 4.39 (s, 2H); 4.10 (s, 2H);1.17 (s, 6H). LC-MS: 182.31 (M+l).

The synthetic route of tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate has been constantly updated, and we look forward to future research findings.

Electric Literature of 54605-72-0, 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. 54605-72-0, name is 1-Phenylpyrazole-4-carboxaldehyde, This compound has unique chemical properties. The synthetic route is as follows.

Step 2: A solution of 4-(Piperazin-1 -yl)quinazoline (1.0 g, 4.7 mmol) and 1 -phenyl-1 H-pyrazole- 4-carbaldehyde (0.81 g, 4.7 mmol) in 1 ,2- dichloroethane (20 ml.) was treated with sodium triacetoxy borohydride (1.5 g, 7 mmol) and the reaction mixture was stirred overnight. The mixture was diluted with dichloromethane (30 ml.) and washed sequentially with 25 ml. portions of 1 M NaOH, water and brine. The organic layer was evaporated and the desired product was purified by column chromatography on silica gel column using ethyl acetate/hexane (10-50%) as the mobile phase the desired product was obtained as a white solid (1.5 g). Mass Spec, M+H = 371.

The chemical industry reduces the impact on the environment during synthesis 1-Phenylpyrazole-4-carboxaldehyde. I believe this compound will play a more active role in future production and life.

Application of 112029-98-8, 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. 112029-98-8, name is (1-Methyl-1H-pyrazol-4-yl)methanol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

[00775] Compound 58-a was synthesized according to Method A. Amide 58-b was synthesized from compound 58-a and 2-aminopyrazolo[ 1 ,5-a]pyrimidine-3-carboxylic acid according to Method D. Potassium teftbutoxide (0.25 mmol, 1.5 equiv was then suspended in anhydrous tetrahydrofuran (1 mL). A solution of (1-methyl- 1H-pyrazol-4-yl)methanol in tetrahydrofuran (1 mL) was then added and the mixture was heated to 40 ¡ãC. A solution of compound 58-b (0.17 mmol, 1.0 equiv) in tetrahydrofiaran (1 mL) was added and the temperature was increased to 60 ¡ãC. The reaction was heated for 45 mm after which there was no more starting material by LC/MS analysis. The mixture was cooled and poured into brine and then extracted with ethylacetate (2x). The combined organic layers were dried and concentrated onto silica gel (2g). The residue was then purified using flash silica gel chromatography (ISCO, Si-i 2g column, gradient of 0-10percent methanol, methylene chloride). The product containing fractions were then concentrated and further purified using reverse phase HPLC (Interchim-sunfire, gradient of 5- 50percent acetonitrile water, ammonium bicarbonate buffer) to provide compound 67 as the desired product. ESI-MS m/z: 535.4 [M+H]+.

The synthetic route of (1-Methyl-1H-pyrazol-4-yl)methanol has been constantly updated, and we look forward to future research findings.