Day: January 7, 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. 1613191-73-3, name is Allyl 3,5-diamino-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., category: pyrazoles-derivatives

To a suspension of allyl 3,5-diamino-1H-pyrazole-4-carboxylate 3 (42.72 g, 234.5 mmol) in DMSO (270.8 mL)/Water (270.8 mL), was added p-TsOH hydrate (46.72 g, 245.6 mmol) and 3-(diisopropylamino)-2-fluoro-prop-2-enal (described in Tetrahedron Letters, 33(3), 357-60; 1992) (38.69 g, 223.3 mmol). The reaction mixture was heated to 100 C. for 3 hr. during which time a solid slowly precipitated out of solution. The orange suspension was allowed to cool down to RT overnight. The solid was filtered, washed with water and dried under vacuum to give allyl 2-amino-6-fluoro-pyrazolo[1,5-a]pyrimidine-3-carboxylate 4 as a sand solid (45.05 g, 85% 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.

Synthetic Route of 5203-77-0, 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. 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, This compound has unique chemical properties. The synthetic route is as follows.

Step 6: Synthesis of 4-(4-chloro-3-ethylsulfinyl-2-methyl benzoyl)-5-hydroxy-1,3-dimethylpyrazole128 mg (1.14 mmol) of 5-hydroxy-1,3-dimethylpyrazole were added to 270 mg (purity 95% by weight; 1.04 mmol) of 4-chloro-3-ethylsulfinyl-2-methylbenzoic acid in 20 ml of dichloromethane (CH2Cl2). 239 mg (1.24 mmol) of 1-(3′-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride were added, and the mixture was stirred at RT for 16 h. For work-up, 3 ml of 1M HCl were added, and the organic phase was freed from the solvent. 210 mg (2.07 mmol) of triethylamine, 10 drops of acetone cyanohydrin and a spatula tip of potassium cyanide were added to the residue in 20 ml of acetonitrile. The reaction mixture was stirred at RT for 16 h and then freed from the solvent. The residue was stirred at RT with 25 ml of a mixture of aqueous saturated sodium bicarbonate solution and diethyl ether for 10 min. The phases were separated, and the aqueous phase was acidified with dilute HCl and then extracted with CH2Cl2. The organic phase was freed from the solvent and the residue was then purified chromatographically. This gave 100 mg of clean product.

The chemical industry reduces the impact on the environment during synthesis 1,3-Dimethyl-1H-pyrazol-5-ol. I believe this compound will play a more active role in future production and life.

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 120068-79-3 as follows. Application In Synthesis of 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile

General procedure: A mixture of compound A (5 mmol) and corresponding benzaldehyde (5 mmol) in 10 mL ethanol was refluxed for 24 hours in a reaction flask wrapped up by silver paper. Upon the reactions completed (monitored by TLC), tawny solids were obtained through suction filtration. The precipitates were washed with ethanol (5 mLx3) and recrystallized from ethanol with 50-84% yields.

According to the analysis of related databases, 120068-79-3, the application of this compound in the production field has become more and more popular.

Application of 73387-46-9,Some common heterocyclic compound, 73387-46-9, name is 3-(4-Bromophenyl)-1H-pyrazole, molecular formula is C9H7BrN2, 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.

Intermediate A4 6-methoxy-2-(4-( 1 -methyl- 1 H-pyrazol-3 -yl)phenyl)-3.4-dihydroisoquinolin- 1 (2H)-one and 6-methoxy-2-(4-(l -methyl- lH-pyrazol-5-yl)phenyl)-3.4-dihydroisoquinolin-l(2H)-one Step 1 : 3-(4-bromophenyl)-lH-pyrazole (0.377 g, 1.690 mmol) was dissolved in THF (8.45 ml). 60% Sodium hydride in oil (0.101 g, 2.54 mmol) was added and the reaction was stirred at rt for 15 min. Methyl iodide (0.116 ml, 1.859 mmol) was added and the reaction was stirred overnight at room temperature. The reaction was quenched with water and extracted three times with dichloromethane. The organic layers were combined, passed through a phase separator and concentrated. The crude material was purified via silica gel chromatography using 0-50% ethyl acetate in heptanes to afford a 2: 1 mixture of products (370 mg, 1.561 mmol, 92 % yield) as a yellow solid. NMR (400 MHz, CHLOROFORM-^ delta ppm 3.86 – 3.95 (m, 3 H), 3.97 (s, 6 H), 6.34 (d, J=1.52 Hz, 1 H), 6.54 (d, J=2.02 Hz, 2 H), 7.30 – 7.33 (m, 2 H), 7.40 (d, J=2.53 Hz, 2 H), 7.49 – 7.56 (m, 5 H), 7.59 – 7.64 (m, 2 H), 7.66 – 7.72 (m, 4 H). LC MS (m/z, MH+): 238.9.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(4-Bromophenyl)-1H-pyrazole, its application will become more common.

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. 52867-42-2, name is Methyl 2-methyl-5-oxo-2,5-dihydro-1H-pyrazole-3-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Formula: C6H8N2O3

To a stirred solution of methyl 5-hydroxy-2-methyl-pyrazole-3-carboxylate (0.3 g, 1.92mmol) in DCM (30 mL) at 0 C, Pyridine (0.18 g, 2.30 mmol) followed by Tf20 (0.59 g, 2.11mmol) was added dropwise. The reaction mixture was slowly warmed toRT and stirred for 2h (TLC indicated complete consumption of starting material). The reaction mixture wasslowly diluted with water (15 mL) and extracted with DCM (2 x 30 mL). The combinedorganic extracts were washed with brine (25 mL), dried over Na2S04 and concentrated underreduced pressure to afford methyl 2-methyl-5-(trifluoromethylsulfonyloxy)pyrazole-3-carboxylate (580 mg, 93% ), which was carried to the next step without further purification.LCMS: m/z: 289.4 [M+Ht.

The synthetic route of 52867-42-2 has been constantly updated, and we look forward to future research findings.

Application of 3994-50-1,Some common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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: 80% hydrazine hydrate (1 mL) and 10% palladium charcoal (0.04 g) were added to a solution of 2a (2 mmol) in ethanol (5 mL). The reaction was hated to 80C for 10 min and filltered by celite. The filtrate was dried by sodium sulfate, and concentrated in vacuum to afford compound 3a, which were used without further purification.

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

28466-26-4, name is 4-Aminopyrazole, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 4-Aminopyrazole

lH-Pyrazol-4-amine (10.4 g, 125 mmol) was dissolved in concentrated HCl (36.8 mL)/water (186 mL) and cooled to 0C. A solution of sodium nitrite (9.05g, 131 mmol) in water (122 mL) was added dropwise while maintaining the internal temperature below 4C. On complete addition, the mixture was stirred at 0C for 30 min. The resulting diazonium chloride solution was added via a pipette to a solution of tert-butyl acetoacetate (21.8 mL, 131 mmol) and sodium acetate (124 g, 1.51 mol) in water (122 mL) and EtOH (122 mL) at 0C. The resulting mixture was stirred between 0-1 C for two hours. The solid was filtered and dried in-vacuo to afford terf -butyl 3-oxo-2-[lH-pyrazol-4-yldiazenyl]butanoate as a yellow-brownish powder. LRMS (ESI) calc’d for CI 1Eta17Nu403 [M+H]+: 253, Found: 253.

The synthetic route of 28466-26-4 has been constantly updated, and we look forward to future research findings.

Electric Literature of 180207-57-2, 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 180207-57-2 as follows.

A mixture of thionyl chloride (6.318 g, 53.55 mmol) and 2-(1H-pyrazol-4-yl)ethan-1-ol (2.0 g, 17.85 mmol) was heated to 70C for 15 minutes. The reaction mixture was concentrated under reduced pressure, the residue was triturated with ethanol/diethyl ether to the title compound (2.3 g, 98%) as an off-white solid. (0690) LC-MS (method 9): f = 1.61 min; m/z = 131.06 (M+H-).

According to the analysis of related databases, 180207-57-2, the application of this compound in the production field has become more and more popular.

Application 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 1 1,5-Dimethyl-1H-pyrazol-3-amine (400 mg, 3.6 mmol, Eq: 1.00) and 4-bromo-6-chloro-2-methylpyridazin-3(2H)-one (965 mg, 4.32 mmol, Eq: 1.20) were combined with 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (312 mg, 540 mumol, Eq: 0.15), cesium carbonate (3.52 g, 10.8 mmol, Eq: 3) and tris(dibenzylideneacetone)dipalladium(0) (165 mg, 180 mumol, Eq: 0.05) in dioxane (10.0 ml). The solution was degassed with Ar. The reaction mixture heated at 100 C. for 18 h. The mixture was cooled to room temperature. The solution was diluted with 100 ml DCM. The organic layer was washed with water. The organic layer was dried over MgSO4. Concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 40 g, 10% to 50% (60:10:1 DCM:MeOH:NH4OH)/DCM gradient) to give 6-chloro-4-(1,5-dimethyl-1H-pyrazol-3-ylamino)-2-methylpyridazin-3(2H)-one (408 mg, 45%). LC/MS-ESI observed [M+H]+ 235.

The synthetic route of 1,5-Dimethyl-1H-pyrazol-3-amine 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. 27006-76-4, name is 5-Chloro-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C6H7ClN2O

General procedure: Toa stirred solution of substituted phenol (75 mmol) in DMF or DMSO (25mL), wasadded solid potassium hydroxide (90 mmol) at room temperature. The resultingmixture was stirred at 45 Cfor 2 h and then 5-chloropyrazole-4-carbaldehyde (5) (50 mmol) was added in portions. The reaction mixture was heatedto 110C. After6-22 h, the mixture was poured into water and extracted with ethyl acetate. Thecombined extracts were dried over anhydrous magnesium sulfate, filtered, andconcentrated to obtain compounds 6a-6z. Then the product 6 (10mmol) was added into a stirred mixture of hydroxylamine hydrochloride(15 mmol) and potassium hydroxide (20 mmol) in methanol or ethanol (30 mL) atthe room temperature. The reaction mixture was refluxed for 5-20 h. Oncompletion, the mixture was poured into water (80 mL), and the solidprecipitate was filtered, washed with water, and dried to afford thecorresponding pyrazole oximes 7a-7z, which were used for the following transformations withoutfurther purification.

According to the analysis of related databases, 27006-76-4, the application of this compound in the production field has become more and more popular.