Day: February 23, 2021

Adding a certain compound to certain chemical reactions, such as: 930-36-9, name is 1-Methylpyrazole, 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 930-36-9, HPLC of Formula: C4H6N2

Step 1 : 4-iodo- l -methyl- lH-pyrazole A mixture of 1 -methy 1-1 H-pyrazole (7) (37 gm, 0.6090 moles), iodine (57. 1 gm, 0.225 moles), hydrogen peroxide (9.2 gm, 0.27 moles) and DI water ( 1 10 ml) were stirred for 24 hour at 20-30C. Progress of the reaction was monitored by HPLC and TLC. The reaction mixture was cooled to 5- 10C. The reaction mixture was quenched with 20% aqueous sodium bisulfite ( 100 ml) and stirred for 1 hour at 5-10C. The solid product obtained was filtered off, washed with cold DI water ( 100 ml) and dried at 40-45C to yield the product, 4-iodo- l – methyl- 1 H-pyrazole. Dry wt : 56 gm Yield : 1.51 w/w (60%)

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-Methylpyrazole, other downstream synthetic routes, hurry up and to see.

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. 113100-53-1, name is 1-Methyl-3-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 113100-53-1

Reference Example 1 1-Methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid (4′-chlorobiphenyl-2-yl) amide A solution of 1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid (0.68 g) and oxalyl chloride (0.49 g) in methylene chloride (30 ml) is stirred for 2 hours at room temperature in the presence of a catalytic amount of DMF. The resulting acid chloride solution is then added to a solution of 4′-chlorobiphenyl-2-ylamine (0.71 g) and triethylamine (0.36 g) in 15 ml of methylene chloride at 0C. The reaction mixture is then stirred for 4 hours at room temperature. After distilling off the solvent in a water-jet-vacuum, the residue is taken up in ethylacetate/water. The ethylacetate phase is extracted twice with water. After drying of the organic phase with Na2SO4, the solvent is distilled off in a water-jet-vacuum and the residue purified by column chromatography (silica gel; eluant: ethylacetate/hexane=1:1). 0.8 g of 1-methyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid (4′-chlorobiphenyl-2-yl) amide are obtained in the form of slightly brownish crystals having a melting point of 144-146C.

According to the analysis of related databases, 113100-53-1, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 288-13-1, name is 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 288-13-1, Application In Synthesis of 1H-Pyrazole

Example 55:; N-[6-(2-Isopropyl-2H-pyrazol-3-yl)-2,4-dioxo-7-trifluoromethyl-l,4-dihydro-2H- quinazolin-3-yl]-methanesulfonamide; 1 -Isopropy 1- 1 H-pyrazole; A mixture of pyrazole (5 g, 73.44 mmol), NaHCO3 (12.2 g, 2 eq) and 2-bromopropane (15 mL, 2eq) was stirred at 1200C for 90 h. Over this period, 2-bromopropane was added when necessary to keep an adequate volume. The solids were removed by filtration and the resulting solution was distillated. From the distillation, a colorless syrup (4.6 g, bp 1480C, 57%) was collected..

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Reference of 71229-85-1, These common heterocyclic compound, 71229-85-1, name is 4-Bromo-1-ethyl-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.

[0511j A solution of (6-bromo- i-ethyl-S -fluoro- 1 H-benzo [d]imidazol-2- yl)diphenylmethanol (0.21 g, 0.50 mmol), 4,4,4?,4?,S ,S ,S?,S?-octamethyl-2,2?-bi( 1,3,2- dioxaborolane) (0.25 g, 1.0 mmol), i,i?-bis(diphenylphosphino)ferrocenepalladium(II) dichloride (0.035 g, 0.050 mmol) and potassium acetate (0.098 g, 1.0 mmol) in dioxane (10 mL) was stirred at reflux for 5 hours. After cooling to ambient temperature, 4-bromo-i-ethyl- 1H-pyrazole (0.088 g, 0.5 mmol), tetrakis(triphenylphosphine)palladium (0) (0.055 g, 0.05 mmol), cesium carbonate (0.33 g, 1.0 mmol) and water (3 mL) were added. The reaction mixture was stirred at 100 C for 12 hours. After cooling to ambient temperature, ethyl acetate and water were added. The organic layer was separated, washed with brine, dried (sodium sulfate), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel to give (i-ethyl-6-(i-ethyl-1H-pyrazol-4-yl)-5-fluoro- 1H-benzo[d]imidazol-2-yl)diphenylmethanol (0.10 g, 45%) as solid. LCMS ESI (+) mlz 441 (M+H).

The synthetic route of 71229-85-1 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. 64781-79-9, name is 4-Methyl-1H-pyrazol-3-amine, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Methyl-1H-pyrazol-3-amine

EXAMPLE 3 3-Methyl-7-(3-pyridyl)pyrazolo[1,5-a]pyrimidine As for Example 2, 3-amino-4-methylpyrazole is heated at reflux temperature for 6 hours with 3-dimethylamino-1-(3-pyridyl)-2-propen-1-one in glacial acetic acid to give the product of the example.

The synthetic route of 64781-79-9 has been constantly updated, and we look forward to future research findings.

Related Products of 31037-02-2, 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. 31037-02-2, name is Ethyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

2 g of the starting material 1-methyl-5-amino-4-ethoxycarbonylpyrazole was dissolved in 30 mL of tetrahydrofuran at room temperature and stirred to dissolve. Further, 5.2 g of triphenylmethane bromide was added, and after stirring and dissolving, 1.5 g of triethylamine was further added dropwise, and after heating, the temperature was gradually raised to 40 C.The mixture was stirred and condensed for 2.5 hours, and solids were precipitated during the reaction. After the reaction was finished, the reaction solution was gradually cooled to about 0 C.After stirring for 1 hour, the reaction solution was filtered to remove the salt component.The filter cake was washed again with 5 mL of tetrahydrofuran.A solution of the corresponding intermediate compound of formula III in tetrahydrofuran is finally obtained, which is ready for use.

The synthetic route of Ethyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate has been constantly updated, and we look forward to future research findings.

Related Products of 78703-53-4,Some common heterocyclic compound, 78703-53-4, name is 1,3-Dimethyl-1H-pyrazole-4-carboxylic acid, molecular formula is C6H8N2O2, 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: 1,3-Dimethyl-1H-pyrazole-4-carboxylic acid of formula (III) (7.76 g, 40 mmol)Reflowed with thionyl chloride (47.6 g, 0.4 mol) for 4 hours.When the reaction system turns into a pale yellow transparent liquid,Continue to react for 30 minutes,The reaction stops,After cooling to room temperature, it was distilled under reduced pressure.1,3-dimethyl-1H-pyrazole-4-yl chloride,1,3-Dimethyl-1H-pyrazole-4-yl chloride (2mmol)Add 15ml of dichloromethane,Join(R)-1-phenethyl-1-amine(2.1mmol),Then triethylamine (0.3 g, 3 mmol) was slowly added dropwise at room temperature overnight;TLC (EA: PE=2:1(V)) tracking,After the reaction was completed, it was extracted three times with a dichloromethane/water = 1:1 (V) system.Concentrated organic layer,Extracted with toluene or 75% ethanol,Column chromatography (EA: PE = 2:1 (V)),Obtained (K19)(R)-1,3-dimethyl-N-(1-phenethyl)-1H-pyrazole-4-carboxamide;

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

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. 2075-46-9, name is 4-Nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., Computed Properties of C3H3N3O2

To a solution of 4-nitro- 1 H-pyrazole (5.0 g, 44.2 mmol) in CH3CN (100 ml) was added 1 -bromo-2-methoxyethane (4.15 ml, 44.2 mmol, 4.15 mL) and K2C03 (12.22 g, 88.4 mmol). The mixture was stirred at 80 C for 12 h. The solvent was removed under reduced pressure. The residue was diluted with water (30 ml) and extracted with EtOAc (3 x 50 ml), the organic layers were combined and washed with brine (20 ml), dried over Na2S04, and concentrated. The resulting residue was purified by FCC (10 – 25 % petroleum ether in ethyl acetate) to give the title compound as a colourless oil (Y = 79 %). H NMR (400 MHz, chlorofomwf) d ppm 8.24 (s, 1H), 8.08 (s, 1H), 4.32 (t, J= 5 Hz, 2H), 3.75 (t, J= 5 Hz, 2H), 3.36 (s, 3H).

The synthetic route of 2075-46-9 has been constantly updated, and we look forward to future research findings.

Electric Literature of 5334-39-4, A common heterocyclic compound, 5334-39-4, name is 3-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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 -methyl -4-nitro-lH-pyrazole (5 g, 39.34 mmol) in DMF (50 rnL) was added NaH (1.89 g, 47.21 mmol, 60% purity) at 0 C under N2. The mixture was stirred at 20 C for 1 h, then added with ethyl 2-chloropropanoate (10.75 g, 78.68 mmol, 10.05 mL) and stirred for 15 h. The mixture was poured into ice water (250 mL). The aqueous phase was extracted with EtOAc (3 chi 100 mL). The combined organic phase was washed with brine (3 chi 100 mL), dried over anhydrous NaaS&t, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (PE:EtOAc = 2: 1), to give a mixture of ethyl 2-(5-methyi-4-nitro-pyrazoi-l-yl)propanoate and ethyl 2-(3- methyl-4-nitro-pyrazol-l-yl)propanoate as a yellow oil LCMS: RT 0.745 min, m/z = 228.2 [M+H]+ To a mixture of ethyl 2-(5-methyl-4-nitro-pyrazol-l -yl)propanoate and ethyl 2-(3-methyl-4-nitro- pyrazol-l-yl)propanoate (9.3 g, 40.93 mmol) in MeOH (90 mL) was added NaBH4 (3.87 g, 102.33 mmol) at 0 C under N2. The mixture was stirred at 0 C for 2 h. The mixture was concentrated under reduced pressure and purified by silica gel column chromatography (PE:EtOAc = 3: 1), to give a mixture of 2-(5- methyl-4-nitro-pyrazol- l-yl)propan-l -ol and 2-(3-methyl-4-nitro-pyrazol-l-y])propan-l-ol was obtained as a yellow solid. LCMS: RT 0.707 mm, m/z = 222.1 [M+H]+ To a solution of 2~(5 -methyl – -nitro- pyrazol-l-y])propan-l-ol, 2-(3-methyl-4-nitro-pyrazol-l-yl)propan-l-ol (2.08 g, 1 1.23 ramol) and Cul (428 mg, 2.25 mmol) in CCN (20 mL) was added a solution of 2,2-difluoro-2-fluorosulfonyl-acetic acid (3 g, 16.85 mmol, 1.74 mL) in CH3CN (10 mL) dropwise at 55C over a period of 30 min under N2. The reaction mixture was stirred at 55 C for 2.5 h. The mixture was concentrated under reduced pressure and purified by silica gel column chromatography (PE:EtOAc = 6: 1), to give a mixture of l-[2- (difluoromethoxy)-l -methyl-ethyl]-5-methyl-4-nitro-pyrazole and l-[2-(difluoromethoxy)-l-methyl- ethyi]-3-methyl-4-nitro-pyrazoie was obtained as a yellow oil. LCMS: RT 0.758 min, m/z = 236.52 i H | .To a mixture of l-[2- (ditluoromethoxy)-l-methyl-ethyl]”5-methyi-4-nitro-pyrazole and l-j2-(difiuoromethoxy)-l -methyl – ethyl]-3 -methyl -4 -nitro-pyrazole (760 mg, 3.23 mmol) in EtOH (20 mL) was added Fe (902.38 mg, 16.15 mmol) and NH4CI (864 mg, 16.15 mmol, 564.87 ,uL). The mixture was stirred at 80C for 2 h. The mixture was cooled to 20 C and concentrated under reduced pressure. The residue was poured into ice water (10 mL). The aqueous phase was extracted with EtOAc (3 x 10 mL). The combined organic phase was washed with brine (10 mL), dried over anhydrous NazSC^, filtered and concentrated under reduced pressure, to give a crude l-[2~(difiuoromethoxy)-l~methyl-ethyl]~5-methyi-pyrazol-4-amine and l-[2- (difluoromethoxy)-l-methyl-ethy]]-3-methyl-pyrazol-4-amine, which was used into the next step without further purification. LCMS: RT 1.026 min, nv’z = 186.1 | M ¡¤ 1 1 | To a mixture of 2-chloro-N-methyl-5-(trifluoromediyl)pyrimidin-4-ainine (372 rng, 1.75 mmol), l-[2- (difiuoromethoxy)- 1 -methyl-ethyl] -3 -methyl -pyrazol-4-amme and 1 – [2-(difluoromethoxy)- 1 -methyl – ethyi]-5-methyl-pyrazol-4-amine (300 mg, 1.46 mmol) in 1,4-dioxane (10 mL) was added TEA (295 mg, 2.92 mmol, 404.75 muTau) in one portion under N2. The mixture was stirred at 120 C for 2 h . The mixture was concentrated under reduced pressure. The residue was purified by prep-HPLC (FA). N2-[l-[2-(difluoromethoxy)-l-methyl-ethyl]-5-methyl-pyrazol-4-yl]-5-(difluoromethyl- fluoranyl)-N4-methyl^yrimidine-2,4-diamine (D-48): [H NMR (400 MHz, CDC M: delta 8, 10 (s, 1 H), 7.85 (br. s., 1 H), 6.62 (br, s, 1 H), 5.86 – 6.31 (m, 1 I I). 5.14 (br. s., 1 H), 4,44 – 4.55 (m, 1 H), 4.22 (t, J=9,48 Hz, 1 H), 4.08 (dd, J=10.36, 5.07 Hz, 1 H), 3.00 (d, ,7=4.85 Hz, 3 H), 2.18 – 2.30 (m, 3 H), 1.53 (d, ,7=7.06 Hz, 3 H): HPLC: RT 1.94 mm; MS: m/z = 381.1 j M ‘N2-[l-[2-(difluoromethoxy)-l-methyl-ethyl]-3-methyl-pyrazol-4-yl]-N4-methyl-5- (trifluoromethyl)pyrimidine-2, -diamine (D-21): NMR (400 MHz, CDC13): 5 8.12. (br. s., 1 H), 7.92 (br. s? 1 H), 6,97 (br. s, 1 H), 5.88 – 6.38 (m, 1 H), 5.21 (br. s? 1 H), 4,47 (d, .7=5,52 Hz, 1 H), 3.99 – 4,20 (m, 2 H), 3.06 (d, J=2.89 Hz, 3 1 1). 2.26 (s, 3 H), 1.56 (d, ,7=6.78 Hz, 3 H). HPLC: RT 1.93 mm; MS: m/z: 381.1 [M4-H]+.

The synthetic route of 5334-39-4 has been constantly updated, and we look forward to future research findings.

Related Products of 175137-46-9,Some common heterocyclic compound, 175137-46-9, name is 5-Cyclopropyl-1H-pyrazol-3-amine, molecular formula is C6H9N3, 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.

The solution of 3,5-difluoro-2-nitrobenzonitrile (Method 16; 5.80 g, 31.5 mmol), 5- cyclopropyl-lH-pyrazol-3-amine (4.66 g, 37.8 mmol) and DIEA (5.5 ml, 31.5 mmol) in THF (100 ml) was stirred at 25 C for 20 hours. The solvent was removed under reduced pressure and the residue was purified by chromatography (DCM-EtOAc = 10 : 1) to give the title compound as a yellow solid (5.50 g, 61%). NMR (400 MHz) 12.43 (s, 1H), 9.70 (s, 1H), 8.22 (d, J = 12.0 Hz, 1 H), 7.51 (d, J = 5 .2 Hz, 1 H), 5 .92 (s, 1 H), 1.89 (m, 1 H), 0.95 (m, 2H), 0.71 (m, 2H). Rt 3.19 min. MS: Calcd. : 287; Found: [M+H]+ 288.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 5-Cyclopropyl-1H-pyrazol-3-amine, its application will become more common.