Month: March 2021

Synthetic Route of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

200 mg (0.71 mmol) of 2-methyl-3-methylsulfonyl-4-trifluoromethylbenzoic acid together with 87 mg (0.78 mmol) of 5-hydroxy-1,3-dimethylpyrazole and a catalytic amount of 4-N,N-dimethylaminopyridine were initially charged in 20 ml of dry CH2Cl2, and 163 mg (0.85 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added. The mixture was stirred at RT for 3 h, and 3 ml of 1 M HCl were then added. After phase separation, the aqueous phase was extracted with CH2Cl2. The organic phases were dried and concentrated. The residue was taken up in 20 ml of acetonitrile and 143 mg (1.42 mmol) of triethylamine, and eight drops of acetone cyanohydrine and a spatula tip of KCN were added. The mixture was stirred at RT for 16 h and concentrated. 15 ml of CH2Cl2 and then 2 ml of 1M HCl were added to the residue. After phase separation, the aqueous phase was extracted with CH2Cl2. The combined organic phases were dried and concentrated. The residue was purified chromatographically. What was isolated were 112.7 mg of pure product.

The synthetic route of 1,3-Dimethyl-1H-pyrazol-5-ol has been constantly updated, and we look forward to future research findings.

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. 37622-90-5, name is Ethyl 4-pyrazolecarboxylate, A new synthetic method of this compound is introduced below., Formula: C6H8N2O2

To a solution of ethyl 1H-pyrazole-4-carboxylate (31 g) and sodium acetate (120 g) in a mixed solvent of ethanol (200 mL) and water (300 mL) was added bromine (140 g), and the mixture was stirred at room temperature for 10 hr. To the reaction mixture was added sodium thiosulfate (180 g), and the mixture solvent was evaporated under reduced pressure. The reaction mixture was poured into water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (65 g). (1090) MS (ESI+): [M+H]+ 296.7

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.

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. 35691-93-1, name is Ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: 35691-93-1

General procedure: 4.3.1. Ethyl 5-amino-2-methylpyrazolo[1,5-a]quinoline-3-carboxylate (7a). Condition C: A mixture of 2-fluorobenzonitrile6a (121 mg, 1.00 mmol), 1H-pyrazole 4 (202 mg, 1.20 mmol) andCs2CO3 (980 mg, 3.00 mmol) in DMF (5.0 mL) was stirred at 120 Cfor 16 h. After monitoring the end of the reaction on TLC, themixture was cooled to room temperature and diluted with water.The resulting mixture was extracted with ethyl acetate twice. Thecombined organic layers werewashed with water twice, dried overMgSO4 and the solvent was removed in vacuo to afford a residue.The residue was purified by flash column chromatography(hexane:EtOAc1:1) on silica gel to afford 7a (124 mg, 46% yield).Condition D: The reaction was carried out in DMSO instead of DMFunder the same conditions as that of condition C to afford 7a (175 mg, 65% yield).

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 82560-12-1, These common heterocyclic compound, 82560-12-1, name is 3-Amino-5-tert-butylpyrazole, 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.

To a solution of 3-(tert-butyl)-lH-pyrazol-5-amine (1.00 g, 7.20 mmol) in toluene (13 mL) was added 5-bromo-2-fluorophenol (1.51 g, 7.90 mmol), potassium carbonate (2.08 g, 15.1 mmol), (IS, 2S)-N,N’-bis-methyl-l,2-cyclohexane-diamine (0.20 g, 1.40 mmol) then copper (I) iodide (0.07 g, 0.36 mmol). The mixture was degassed then heated at 150 C for 1 h using microwave irradiation. Another portion of copper (I) iodide (0.07 g, 0.36 mmol) was added and the reaction mixture heated at 150 C for a further 1 h using microwave irradiation. The mixture was diluted with EtOAc and water and the phases separated. The aqueous layer was then extracted with EtOAc (2 x). The combined organic layers were washed with brine, dried (Na2S04), filtered and evaporated in vacuo to give an impure solid. The residue was partitioned between DCM and water and the phases separated. The organic layer was evaporated in vacuo and the residue was purified by FCC, using 0-5% MeOH in DCM. Further purification by FCC, using 0-25% EtOAc in DCM, gave the title compound as an orange gum (1.25 g, 70%>). LCMS (Method 3): Rt 2.33 min, m/z 250.3 [MH+].

Statistics shows that 3-Amino-5-tert-butylpyrazole is playing an increasingly important role. we look forward to future research findings about 82560-12-1.

Electric Literature of 14531-55-6, 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. 14531-55-6, name is 3,5-Dimethyl-4-nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

DIAD (837muIota_, 4.25mmol) was added to a solution of 3-methyl-4-nit.ro- 1 H-pyrazole (500mg, 3.54mmol), /V-methyl-4-piperidinol (408mg, 3.54mmol) and triphenylphosphine (860mg, 4.25mmol) in THF (25ml_). The reaction mixture was stirred at rt for 5 days. The mixture was cone, in vacuo before purification by flash chromatography on silica, washing with DCM, then 30%, 70%, 100% EtOAc/DCM mixtures. The product was eluted with 5%, 10% then 20% MeOH/DCM to give the title compound as an off-white crystalline solid (289mg, 34%). LCMS (Method 1 ) Rt 2.721 min, ESIMS m/z [M+H]+ 239.3.

The synthetic route of 3,5-Dimethyl-4-nitro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Reference of 151049-87-5, 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 151049-87-5 as follows.

A 30m1 tube was charged with ethyl N-(diphenylmethylene)glycinate (2.5 g, 9.35 mmol), 3-bromo-1-methyl-lh-pyrazole (1.51 g, 9.35 mmol), potassium phosphatetribasic (6 g, 27.7 mmol) in toluene (15 mL) and the mixture was purged with N2 for 5 minutes. Bis(tri-tert-butylphosphine)palladium(0) (526 mg, 1.03 mmol) was added and the vial was capped and the mixture was stirred at 100C for 16 hours. The mixture was cooled and filtered over decalite. The filtrate was concentrated in vacuo. The residue was purified by column chromatography using a gradient from 0 till 100% EtOAc inheptane. The product fractions were concentrated in vacuo to yield ethyl2-(benzhydrylideneamino)-2-( 1 -methylpyrazol-3 -yl)acetate (1.95 g) as a pale yellow oil.

According to the analysis of related databases, 151049-87-5, the application of this compound in the production field has become more and more popular.

Reference of 1904-31-0, These common heterocyclic compound, 1904-31-0, name is 1-Methyl-1H-pyrazol-3-amine, 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: To a solution of benzoic acid which was obtained by hydrolysis of methyl esters 8 or 12A-E (0.22 mmol, 1.0 equiv), aminothiazole or imidazo[1,2-a]pyrazin-8-amine or aminopyrazole (0.33 mmol, 1.5 equiv), HATU (0.33 mmol, 1.5 equiv) and HOAt (0.33 mmol, 1.5 equiv) in DMF (2 mL) was added dropwise di(isopropyl)ethylamine (DIPEA) (0.12 mL, 0.67 mmol, 3 equiv). The reaction was run under microwave at 60 ¡ãC (40 W) for 30 min, and then cooled to room temperature and poured into brine. The aqueous layer was extracted with EtOAc. The combined organic layers were washed with brine, dried over anhydrous NaSO4 and concentrated. The residue was purified by chromatography (SiO2, petroleum ether/EtOAc = 4:1-1:1) to yield corresponding amides as white or yellow powder.

The synthetic route of 1904-31-0 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. 398491-59-3, name is tert-Butyl 3-amino-4,6-dihydropyrrolo[3,4-c]pyrazole-5(1H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of tert-Butyl 3-amino-4,6-dihydropyrrolo[3,4-c]pyrazole-5(1H)-carboxylate

To the product from Step A (133 mg) in dichloromethane (3 mL) at 0 0C was added N,N- dnsopropylethylamine (0 21 mL) followed by benzyl chloroformate (0 1 mL) The reaction mixture was stirred at 0 0C for 90 mm, then diluted with dichloromethane (10 mL) and poured into saturated aqueous sodium bicarbonate solution The layers were separated and the aqueous phase extracted with dichloromethane (3×10 mL). The combined organic phases were d?ed over anhydrous sodium sulfate, filtered and evaporated in vacuo The residue was purified on a Biotage Horizon system (silica gel, 0 to 80% ethyl acetate/hexanes gradient) to give the title compound LC/MS 359 3 (M+l)

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 398491-59-3.

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. 1572-10-7, name is 3-Amino-5-phenylpyrazole, This compound has unique chemical properties. The synthetic route is as follows., name: 3-Amino-5-phenylpyrazole

General procedure: N,N-Diisopropylethylamine (3.0-4.0 eq) was added to 8-methoxyquinoline-3-carboxylic acid (1.0 eq) in solvent (dichloromethane, tetrahydrofuran,or N,N-dimethylformamide, 0.05 to 0.2 M) at room temperature. Then, 1-((dimethylamino)(dimethyliminio)methyl)-1H-[1,2,3]triazolo[4,5-b]pyridine 3-oxide hexafluorophosphate(V)(1.0-1.5 eq) was added and the reaction mixture was stirred for five minutes. Then, amine (1.0 – 2.0 eq) was added and the reaction mixture was stirred for one to sixteen hours. 10% Aqueous citric acid was added and the reaction mixture was extracted with dichloromethane, washed with saturated sodium bicarbonate, dried over magnesium sulfate, filtered,and concentrated. The resulting residue was purified by RP HPLC or silica gel chromatography to give the quinoline-3-carboxamide (1%-95% yield).

According to the analysis of related databases, 1572-10-7, the application of this compound in the production field has become more and more popular.

Synthetic Route of 13808-64-5, The chemical industry reduces the impact on the environment during synthesis 13808-64-5, name is 4-Bromo-3-methylpyrazole, I believe this compound will play a more active role in future production and life.

(1) Combine 16.1 g (0.1 mol) of 4-bromo-3-methyl-1H-pyrazole, 10.1 g (0.12 mol) of 3,4-dihydro-2H-pyran, and 0.7 g (0.006 mol) of trifluoroacetic acid ) Add to the reaction bottle and stir to heat to micro-reflux for 12 hours. The reaction formula is as follows:Cool to room temperature, add 0.24 g (0.006 mol) of sodium hydride to neutralize the reaction system,Vacuum distillation to obtain intermediate4-bromo-3-methyl-1- (tetrahydro-2H-pyran-2-yl) -1H-pyrazole and4-bromo-5-methyl-1- (tetrahydro-2H-pyran-2-yl) -1H-pyrazole total 24 grams,The presence of isomers does not affect the next reaction. (2) The intermediates obtained in step (1) 4-bromo-3-methyl-1- (tetrahydro-2H-pyran-2-yl) -1H-pyrazole and 4-bromo-5- Methyl-1- (tetrahydro-2H-pyran-2-yl) -1H-pyrazole 24 g was dissolved in 200 ml of THF, cooled to minus 75 degrees, and n-butyl with a concentration of 2.5 mol / L was added dropwise 48 ml (0.12 mol) of lithium solution, maintaining the temperature at minus 75 degrees Celsius, dropping and holding for half an hour, then adding 14 g (0.12 mol) of N-formylmorpholine at this temperature, the reaction formula in step (2) is as follows :After the reaction is completed, naturally warm to room temperature, add dilute sulfuric acid to quench until the system pH value is less than 1, stir at room temperature for 3-4 hours, neutralize with sodium bicarbonate, extract with ethyl acetate, dry and concentrate to obtain the target product by adsorption and purification on silica gel 3-Methyl-1H-pyrazole-4-carbaldehyde 8 g.The yield of the target product 3-methyl-1H-pyrazole-4-carbaldehyde in this example was 72.7%. 2 is the nuclear magnetic resonance spectrum of the product 3-methyl-1H-pyrazole-4-carbaldehyde obtained in this example;

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, 4-Bromo-3-methylpyrazole, other downstream synthetic routes, hurry up and to see.