Day: March 3, 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. 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid, A new synthetic method of this compound is introduced below., Recommanded Product: 5334-40-7

4-Nitropyrazole-3-carboxylic acid (7.3 g; 15.9 mmol) was added to a stirred solution of 4-amino-1-Boc- piperidine (10.2 mg; 51 mmol), EDC (10.7 g; 55.8 mmol), and HOAt (55.8 g; 19.1 mmol) in DMF (100 ml), and then stirred at room temperature overnight. The solvent was removed by evaporation under reduced pressure and the residue triturated with water (250ml). The resultant cream solid was collected by filtration, washed with water then dried under vacuum to give 13.05 g of 4-[(4-nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1- carboxylic acid tert-butyl ester (LC/MS: Rt 2.50, [M+H]+ 340).

The synthetic route of 5334-40-7 has been constantly updated, and we look forward to future research findings.

Electric Literature of 37622-90-5, 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. 37622-90-5, name is Ethyl 4-pyrazolecarboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a solution of O-methyl-nu-oxide salt intermediate in AcCN (10 ml) obtained as above from 1.37 g (4.71 mmol) N-oxide m-CBA salt and dimethylsulfate (0.49 ml, 1.05 eq.) was added a solution OfNH3 in dry MeOH (7M, Aldrich, 15 ml) under cooling in an icebath. The brown mixture was stirred in a sealed vial at 70 0C overnight. After evaporation of the solvent and aq. workup as above, the crude was purified by silica gel chromatography to give a light-brown, cryst. solid. HR-MS calculated for [MH]+: 134.07127, found: 134.07150.

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

Application of 112029-98-8, These common heterocyclic compound, 112029-98-8, name is (1-Methyl-1H-pyrazol-4-yl)methanol, 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 the solution of alcohol 4b (0.50?g, 2.67?mmol) and DMSO (0.41?g, 5.34?mmol) in ethyl acetate (5?ml) was added ?T3P (1.84?g, 6.68?mmol, 2.5?equiv, 50percent solution in ethyl acetate) at 0?¡ãC. The resulting mixture was allowed to warm to RT and stirred for 1?h. Pyrazine-2-amine 3a (0.254?g, 2.67?mmol) was added to the above mixture and stirred for 15?min, which was followed by the addition of isocyanide 1c (0.33?g, 4.01?mmol) at room temperature and stirring for 4?h. Progress of the reaction was monitored by TLC. After the reaction was complete, the reaction mixture was diluted with ethyl acetate and neutralized with aqueous sodium bicarbonate solution. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (25?mL?¡Á?2), the combined organic phases were washed with water, brine solution, dried over anhydrous sodium sulfate, and concentrated under vacuum to afford a crude product, which was purified on silica gel using ethyl acetate and petroleum ether.

Statistics shows that (1-Methyl-1H-pyrazol-4-yl)methanol is playing an increasingly important role. we look forward to future research findings about 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. 51516-70-2, name is 5-Amino-1-(4-fluorophenyl)-1H-pyrazole-4-carbonitrile belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 51516-70-2

General procedure: (General method). Amixture of the appropriate aminonitrile 1 (3.0 mmol) and1,3-dicarbonyl compound (3.0 mmol) in anhydrous toluene(12 ml) was refluxed for 1 h in a flask equipped with aDean-Stark trap. Tin(IV) chloride (3.0 g, 11.5 mmol) wasadded to the reaction mixture, and refluxing was continuedfor additional 5-6 h. A resinous precipitate was formed,andthe colorless toluene layer was decanted. The residualsolvent was removed on a rotary evaporator, the obtainedglassy solids were dissolved in boiling dioxane, cooled, thenpoured into a solution of Na23 (4.0 g) in water (70 ml).The precipitate that formed was filtered off, washed withwater, dried, and recrystallized from a 5:1 mixture of2-PrOH-DMF.

The synthetic route of 51516-70-2 has been constantly updated, and we look forward to future research findings.

Reference of 27006-76-4, A common heterocyclic compound, 27006-76-4, name is 5-Chloro-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde, molecular formula is C6H7ClN2O, 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.

(3) 8.5 g of 5-chloro-1,3-dimethyl-1H-pyrazole-4-carbaldehyde (0.054 mol)Dissolved in methanol, add Pd / C (0.85g, 0.1w / w) andMgO (1.7g, 0.2w / w);The system was replaced with hydrogen three times;Under the condition of 1 atmosphere of hydrogen,Stir the reaction at 25 C for 16 hours;After the reaction was completed, the solid was removed by filtration (filter cake washing), the filtrate was concentrated under reduced pressure, dissolved in water, and extracted with ethyl acetate.The organic phase was concentrated to obtain 6.3 g of 1,3-dimethyl-1H-pyrazole-4-carbaldehyde as a pale yellow solid; purity 93%, yield 96%.

The synthetic route of 27006-76-4 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. 127107-23-7, name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

Into a 100 mL round-bottom flask under inert atmosphere were placed interemediate 55.1 (200 mg, 0.54 mmol, 1.00 equiv), 2-methylpropan- 2-ol (10 mL), potassium phosphate (346 mg, 1.63 mmol, 3.00 equiv), 1-methyl-1H-pyrazol-4- amine hydrochloride (109 mg, 1.12 mmol, 1.50 equiv), and 3T generation xphos precatalyst (43 mg, 0.05 mmol, 0.10 equiv). The resulting solution was stirred overnight at room temperature. The resulting mixture was concentrated under vacuum and crude was purified using preparative HPLC to furnish 84.4 mg (36%) of compound 1-55 as a pink solid. LCMS (ES, m/z): 430 [M+H] ?H NMR (400 MHz ,CD3OD): oe 7.53 1 (s, 1H), 7.8777.913 (d, 1H), 5.1565.225 (m, 1H), 3.8503.886 (d, 3H), 3.6763.707 (t, 4H), 2.6822.725 (d, 3H), 2.5852.616 (t, 4H), 2.2892.360 (m, 3H), 2.0692.113 (d, 2H), 1.5041.596 (t, 2H), 1.5961.681 (t, 2H).

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.

Synthetic Route of 176969-34-9, 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. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows.

a synthesis reaction experimental device is connected in a circulating cooling reaction pump at 0 C, and nitrogen gas is introduced in the early stage.To remove the air from the reaction flask, keep nitrogen in, and add 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid to the round bottom flask after about 5 minutes.(LM-1-a) 0.528 g (3 mmol), 20 mL of re-distilled dichloromethane,Re-steaming DMF 0.482 mL (6 mmol),The reaction liquid was stirred and 0.316 mL (3.6 mmol) of oxalyl chloride was slowly added dropwise thereto using a dropping funnel. After 1.5h-2.5h reactionThe reaction was closed, and the insoluble material was removed by suction under reduced pressure. The filtrate was slowly added dropwise to a solution of 0.856 g (2.4 mmol) of N-(2-fluorophenyl)-2-aminocyclohexanesulfonamide and 0.6 mL with a dropping funnel. 4.32mmol) triethylamine in a mixed solution of dichloromethane, continue to be lowAfter stirring for 15 min, the reaction was changed to room temperature for about 2 h, and the reaction was monitored by TLC [V (petroleum ether): V (ethyl acetate) = 2:1].During the reaction, the reaction of the raw materials is judged according to the condition of the plate. After the reaction is completed, the reaction is stopped. AdditionalAppropriate amount of methylene chloride, the reaction solution was washed with HCl, washed with NaHCO3, washed with water, dried over anhydrous sodium sulfate, and allowed to stand for more than 8h.The crude product is purified by column chromatography, and the product is recrystallized from dichloromethane or acetone to give a white powdery solid.Pure productN-(2-Trifluoromethyl-4-chlorophenyl)-2-[1-methyl-3-difluoromethyl-4-pyrazolecarboxamido]cyclohexanesulfonamide.

The chemical industry reduces the impact on the environment during synthesis 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid. I believe this compound will play a more active role in future production and life.

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. 2075-45-8, name is 4-Bromo-1H-pyrazole, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Bromo-1H-pyrazole

a) 4-Bromo- 1 -ethyl- 1 H-pyrazoleTo a solution of 4-bromo-l H-pyrazole (5 g, 34 mmol) in DMF were added K2C03 (11.75 g, 85.03 mmol, 2.5 eq.) and iodoethane (8 g, 51 mmol, 1.5 eq.) and the mixture was stirred at RT for 12 h. The mixture was quenched and extracted as in Intermediate Example 5(c). The solvent was distilled off and the crude residue was purified by column chromatography (60-120 silica gel, 40 % ethyl acetate in hexane) to yield the product in 84 % yield (5 g). ? NMR (300 MHz, DMSO-i?): delta 8.02 (s, 1H), 7.55 (s, 1H), 4.15 (q, 2H), 1.37 (t, 3H); LC-MS (ESI): Calculated mass: 175.03;Observed mass: 177.0 [M+H]+ (rt: 0.56 min).

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.

These common heterocyclic compound, 4522-35-4, name is 3-Iodo-1H-pyrazole, 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. Quality Control of 3-Iodo-1H-pyrazole

INTERMEDIATE 29 5-Chloro-4-(3-iodo-lH-pyrazol-l-yl)-2-methoxypyridine A solution of 3-iodo-lH-pyrazole (0.3 g, 1.547 mmol), 5-chloro-2-methoxypyridine- 4-boronic acid (0.377 g, 2.011 mmol), DMAP (0.756 g, 6.19 mmol), copper(II)acetate (0.281 g, 1.547 mmol), and cesium carbonate (1.26 g, 3.87 mmol) in 1,4-dioxane (7.73 mL) was heated at 80 C overnight. The reaction was allowed to warm to room temperature and filtered. The filtrate was diluted with EtOAc and water, and the seperated aq. layer was extracted with EtOAc. The combined organics were dried over MgS04, filtered and concentrated. The residue was purified with flash chromatography (ISCO Combiflash, 24 g, 0-10 % EtOAc in hexanes) to give 5- chloro-4-(3-iodo-lH-pyrazol-l-yl)-2-methoxypyridine, as a white solid. LCMS calc. = 335.93; found = 335.82 (M+H)+. 1H NMR (500 MHz, CDC13): delta 8.25 (s, 1 H); 8.01 (d, J= 2.6 Hz, 1 H); 7.14 (s, 1 H); 6.66 (d, J= 2.5 Hz, 1 H); 3.96 (s, 3 H).

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

Synthetic Route of 15802-80-9, 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. 15802-80-9, name is 3-(tert-Butyl)pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 4 Preparation of 5-[3-(1,1-dimethylethyl)-1H-pyrazol-1-yl]-3-[3-(trifluoromethyl)phenyl]-4-oxazolidinone To a solution of 5-hydroxy-3-[3-(trifluoromethyl)phenyl]-4-oxazolidinone (1 g, 4.05 mmol) in tetrahydrofuran (20 mL) under nitrogen at ~0 C., were added 3-(1,1-dimethylethyl)-1H-pyrazole (0.5 g, 4.05 mmol), triphenylphosphine (1.23 g, 4.7 mmol) and diisopropyl azodicarboxylate (0.88 mL, 4.46 mmol). After the addition, the reaction mixture was allowed to warm up slowly to room temperature and stirred at room temperature overnight. The reaction mixture was then concentrated, and the residue was purified by column chromatography (silica gel, ~20% ethylacetate/80% hexanes) to give a crude product. The crude product was further purified by column chromatography (silica gel, ~20% ethyl acetate/~80% hexanes) to give the title compound, a compound of this invention, as a white solid (14 mg) melting at 95-98 C. 1H NMR (CDCl3): delta 1.26 (s, 9H), 5.57 (d, 1H), 5.79 (d, 1H), 6.08 (s, 1H), 6.20 (d, 1H), 7.45-7.6 (m, 3H), 7.8-7.9 (m, 2H).

The chemical industry reduces the impact on the environment during synthesis 3-(tert-Butyl)pyrazole. I believe this compound will play a more active role in future production and life.