Day: December 22, 2020

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. 141998-92-7, name is 5-Iodo-1-phenyl-1H-pyrazole, A new synthetic method of this compound is introduced below., SDS of cas: 141998-92-7

A) 1-phenyl-5-[(trimethylsilyl)ethynyl]-1H-pyrazole To a solution of 5-iodo-1-phenyl-1H-pyrazole (2.00 g) (J. Org. Chem. 2008, 73, 1, 177-183) in triethylamine (40.0 mL) were added ethynyl(trimethyl)silane (0.80 g), CuT (0.141 g) and PdCl2(PPh3)2 (0.260 g) under an argon atmosphere, and the mixture was stirred at 70 C. for 10 hr. The reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (dichloromethane) to give the title compound (1.54 g). 1H-NMR (400 MHz, CDCl3) delta 0.00 (9H, s), 6.42 (1H, d, J=1.6 Hz), 7.12-7.16 (1H, m), 7.23 (1H, t, J=16 Hz), 7.42 (1H, d, J=1.6 Hz), 7.58-7.60 (2H, m)

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.

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. 930-36-9, name is 1-Methylpyrazole, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 1-Methylpyrazole

General procedure: To a stirred mixture of pyrazole (200 mmol) and the appropriate acid anhydride (350 mmol, 1.75 equiv), concd H2SO4(0.2 mL) was added, and the resulting mixture was stirred under a nitrogen atmosphere in an oil bath until the pyrazole was consumed. For low boiling components, this mixture was heated at reflux. Reaction conditions (temperature and time) are given in Table 2. When the reaction was complete, volatile compounds were removed under reduced pressure and the residue was poured onto 100 mL crushed ice. The reaction mixture was neutralized under vigorous stirring by the addition of 20% aqueous NaOH or (in the case of fluorinated ketones) solid KHCO3 to adjust pH to 7-8. The ketone was extracted with CH2Cl2(3 ¡Á 50 mL) and the combined organic phases were washed with brine (50 mL), dried over MgSO4, and evaporated under reduced pressure. The resulting crude ketone was purified by either distillation or recrystallization from the appropriate solvent.

According to the analysis of related databases, 930-36-9, the application of this compound in the production field has become more and more popular.

Reference of 35344-95-7, 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. 35344-95-7 name is 1H-Pyrazole-4-carbaldehyde, 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 50-mL round-bottom flask was placed a solution of [(ls,3 s)-3 -(3-phenyl- 1 ,2-oxazole-5 -amido)cyclobutyljmethyl 4-methylbenzene- 1 -sulfonate (1g, 2.34 mmol, 1.00 equiv) in DMF (15 mL) then Cs2CO3 (1.5 g, 4.60 mmol, 2.00 equiv) and1H-pyrazole-4-carbaldehyde (338 mg, 3.52 mmol, 1.50 equiv) were added. The resulting solution was stirred for 3 h at 100¡ãC then the solids were removed by filtration. The crude product was purified by Flash-Prep-HPLC (CombiFlash-1: Column, C18 silica gel; mobile phase, X: H20 (0.5percent NH4HCO3), Y: ACN, X/Y=90/10 increasing to X/Y=5/95 within 40 mm;Detector, UV 254 nm) affording 460 mg (56percent) of 3-phenyl-N-[(ls,3s)-3-[(4-formyl-1H- pyrazol-1-yl)methyljcyclobutylj-1,2-oxazole-5-carboxamide as a yellow solid. LCMS (ES, m/z): [M+Hj?= 351.1.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1H-Pyrazole-4-carbaldehyde, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, 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 1280210-79-8, HPLC of Formula: C10H15N3O2

Under N2 protection and a condition free of water and oxygen, Intermediate 2 (1000 mg, 4.78 mmol) was dissolved in N,N-dimethylformamide (15 ml), which was cooled to -15C, and sodium bis(trimethylsilyl)amide (4.78 mL, 2 mol/L, 9.56 mmol) was added, followed by stirring for 30 min, and S-cyclopentylsulfonyl chloride (1.37 g, 8.13 mmol) was added dropwise, followed by reaction for 16 hours at -15C. The temperature was raised to 0C, and the reaction was quenched by addition of water (20 ml) to the reaction solution, which was then extracted with ethyl acetate (20 ml*2). The organic phases were combined, dried over anhydrous sodium sulfate, concentrated, re-dissolved in tetrahydrofuran (20 ml), and cooled to a temperature between -10C and 0C, potassium t-butoxide (85 mg, 0.76 mmol) was added, and the reaction was allowed to proceed for 24 hours at this temperature. After the reaction was completed, a saturated aqueous solution of ammonium chloride (10 ml) and water (10 ml) were added. The solution was extracted with ethyl acetate (20 mL*3). The organic layers were combined, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate (v/v) = 5:1) to obtain a white solid 6a (800 mg, yield 62%).

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, tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 948570-75-0, name is 1-(2-Methoxyethyl)-4-nitro-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. name: 1-(2-Methoxyethyl)-4-nitro-1H-pyrazole

General procedure: 4-nitro-1H-pyrazole (1 equiv), corresponding alcohols (1 equiv) and triphenylphosphine (1.5 equiv) were dissolved in THF, and di-tert-butyl azodicarboxylate (1.5 equiv) was added over approximately 10min. The resulting mixture was stirred at room temperature for 5h and concentrated to dryness. The residue was purified by column chromatography to give intermediates 27a-c. A solution of 4-nitro-1H-pyrazole (1 equiv), potassium carbonate (1 equiv) and the alkylating reagent (1.1 eq) in acetonitrile was heated at 40-80C for 8h. The mixture was diluted with ethyl acetate, and the organic layer was washed with brine, dried over anhydrous Na2SO4 and filtered. The filtrate was concentrated and purified by chromatography to give intermediates 27b-f. Intermediates 27a-f (1 equiv) were dissolved in ethanol, and Pd/C (0.1 equiv) was added. The flask was flushed with H2 and stirred for 3hat 40C. The reaction mixture was filtered through a Celite pad and the filtrate was concentrated to dryness, yielding intermediates 28a-f.

The synthetic route of 1-(2-Methoxyethyl)-4-nitro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 28491-52-3, name is 5-Amino-1H-pyrazol-3(2H)-one, molecular formula is C3H5N3O, 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. Computed Properties of C3H5N3O

A. 1,2,4,7-Tetrahydro-5-methyl-7-(3-nitro-phenyl)-2-oxopyrazolo[1,5,-a]pyrimidine-6carboxylic acid, 1-methylethyl ester A mixture of 3-amino-5-pyrazolone (3.57 g, 36.1 mmole) and 2-[(3-nitrophenyl)methylene]-3-oxobutanoic acid, 1-methylethyl ester (10 g, 36.1 mmole) in dry dimethylformamide (30 ml) was heated at 70 C. under argon for 24 hours. The reaction mixture was allowed to cool to room temperature and then diluted with ether. The resultant precipitate was filtered off and recrystallized from isopropanol to provide 4.23 g of the title A compound in crystalline form, m.p. 254-256 C. Analysis calc’d for C17 H18 N4 O5: C, 56.98; H, 5.06; N, 15.63; Found: C, 57.18; H, 5.10; N, 15.70.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 28491-52-3, its application will become more common.

Synthetic Route of 25016-11-9, 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 25016-11-9 as follows.

Intermediate 69 (600mg, 1 eq.) was dissolved in tetrahydrofuran, and lithium aluminum hydride (210 mg, 1 eq.) was added under ice bath and the mixture was reacted at room temperature for 2 h. After completion of the reaction, 210 mul of water, 210 mul of 10% aqueous sodium hydroxide solution, and 630 mul of water were successively added, followed by addition of anhydrous magnesium sulfate. The mixture was stirred for a while, filtered and evaporated to dryness to give 400 mg of an oil. MS (ESI): 113(M+H)

According to the analysis of related databases, 25016-11-9, the application of this compound in the production field has become more and more popular.

Related Products of 28466-26-4, 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. 28466-26-4 name is 4-Aminopyrazole, 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.

General procedure: A mixture of the appropriate aminopyrazole 1 (0.01 mol), NaN3 (0.78 g, 0.012 mol), andtriethyl orthoformate (1.60 ml, 0.015 mol) or triethylorthoacetate (1.74 ml, 0.015 mol) in glacial acetic acid(10 ml) was stirred for 3-4 h at 90. The reaction mixturewas cooled and poured into ice water (50 ml). In the case ofcompounds 2a-c, 4b, the precipitate that formed wasfiltered off, washed with water, and recrystallized from EtOH. In the case of compounds 2d, 3a, 4a,c, the aqueouslayer was extracted with ethyl acetate (3¡Á15 ml), and theorganic layer was dried over anhydrous Na2SO4. Thesolvent was removed at reduced pressure, and the solidresidue was recrystallized from EtOH.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Aminopyrazole, and friends who are interested can also refer to it.

Electric Literature of 35100-92-6, 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. 35100-92-6, name is 1,5-Dimethyl-1H-pyrazol-3-amine belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Step 7) tert-butyl 4-((5-chloro-2-((1,5-dimethyl-1H-pyrazol-3-yl)amino)pyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate and tert-butyl 4-((2-((1,5-dimethyl-1H-pyrazol-3-yl)amino)pyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate To a suspension of tert-butyl 4-((2,5-dichloropyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate (0.27 g, 0.71 mmol) in anhydrous 1,4-dioxane (6.0 mL) was added 1,5-dimethyl-1H-pyrazol-3-amine (0.16 g, 1.44 mmol), palladium diacetate (32 mg, 0.14 mmol), BINAP (90 mg, 0.14 mmol) and cesium carbonate (0.47 g, 1.43 mmol). The mixture was degassed and refilled with nitrogen for several times in a sealed tube and then stirred under microwave irradiation at 150 C. for 2 hours. The mixture was concentrated in vacuo. The residue was purified by silica gel column chromatography (DCM/a solution of NH3 in MeOH (3M) (v/v)=100/1 to 50/1 to 30/1 to 10/1) to give the tert-butyl 4-((5-chloro-2-((1,5-dimethyl-1H-pyrazol-3-yl)amino)pyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate as a yellow solid (0.19 g, yield 60%), also get tert-butyl4-((2-((1,5-dimethyl-1H-pyrazol-3-yl)amino)pyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate as a brown solid (0.20 g, 67%, impure). For tert-butyl 4-((5-chloro-2-((1,5-dimethyl-1H-pyrazol-3-yl)amino)pyrimidin-4-yl)amino)-3-ethylpiperidine-1-carboxylate LC-MS (ESI, pos. ion) m/z: 450.4 [M+H]+; 1H NMR (400 MHz, CDCl3) delta (ppm): 7.90 (s, 1H), 7.19 (s, 1H), 6.38 (s, 1H), 4.99 (d, J=8.4 Hz, 1H), 4.12-3.91 (m, 3H), 3.67 (s, 3H), 2.93 (t, J=12.0 Hz, 1H), 2.61 (br, 1H), 2.25 (s, 3H), 2.14-2.06 (m, 1H), 1.77-1.66 (m, 1H), 1.48 (s, 9H), 1.45-1.38 (m, 2H), 1.22 (s, 1H), 0.94 (t, J=7.5 Hz, 3H).

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, 1,5-Dimethyl-1H-pyrazol-3-amine, other downstream synthetic routes, hurry up and to see.

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. 25016-20-0, name is 1-Methyl-1H-pyrazole-3-carboxylic acid, A new synthetic method of this compound is introduced below., SDS of cas: 25016-20-0

To a solution of 1 -methyl- 7/-/-pyrazole-3-carboxylic acid (0.100 g, 0.793 mmol), A/,A/-diisopropylethylamine (0.307 g, 2.38 mmol) in tetrahydrofuran (4 ml_) at 20 C was added 1 -[b/s(dimethylamino)methylene]- 7/-/-1 ,2,3-triazolo[4,5-b]pyridinium 3-oxid hexafluorophosphate (0.452 g, 1 .19 mmol). The reaction was stirred for 20 minutes before a solution of 5-(3-chlorobenzyl)pyridin-2-amine (0.173 g, 0.793 mmol) in tetrahydrofuran (1 .0 ml_) was added. The solution was stirred at 20 C for 16 h. The volatiles were removed under reduced pressure and the residue was added to a mixture of dichloromethane (50 ml_) and water (50 ml_). The organic layer was collected, dried over sodium sulfate, filtered and concentrated. The crude sample was dissolved in minimal A/,A/-dimethylformamide and purified via prep-HPLC (Boston C1 8 21 *250 mm 10 pm column; acetonitrile/0.01 % aqueous trifluoroacetic acid) to give A/-(5-(3-chlorobenzyl)pyridin-2-yl)-1 -methyl- 7/-/-pyrazole-3-carboxamide (0.0927 g, 0.285 mmol, 36%) as a white solid. 1 H NMR (400 MHz, Dimethylsulfoxide-c/6) d 9.51 (s, 1 H), 8.29 (s, 1 H), 8.1 0 (d, J = 10.5 Hz, 1 H), 7.88 (d, J = 2.5 Hz, 1 H), 7.71 -7.74 (m, 1 H), 7.23-7.35 (m, 4H), 6.84 (d, J = 2.5 Hz, 1 H), 3.96 (s, 5H); LCMS (ESI) m/z: 327.1 [M+H]+.

The synthetic route of 25016-20-0 has been constantly updated, and we look forward to future research findings.