Tag: M.W=0-100

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. Safety of 1-Methyl-1H-pyrazol-3-amine

A solution of 1 -methyl-1 -/-pyrazol-3-amine (2 g, 20.6 mmol,) in AcOH (50 mL) was treated with 2,5-hexane dione (4.9 g, 43.29 mmol) at ambient temperature under nitrogen atmosphere. The resulting reaction mixture was heated to 100 ¡ãC for 1 h then stirred at ambient temperature for 5 h. The reaction mixture was concentrated under reduced pressure and azeotroped with toluene. The crude product was purified by column chromatography on silica gel using 10percent EtOAc- hexanes eluent to give 3-(2,5-dimethyl-1 H-pyrrol-1 -yl)-1 -methyl-1 H-pyrazole as a liquid (2.5 g, 69percent). 1 H NMR (300 MHz, CDCI3): delta = 7.39 (d, J = 2.1 Hz, 1 H), 6.15 (d, J = 2.4 Hz, 1 H), 5.84 (s, 2H), 3.92 (s, 3H), 2.10 (s, 6H).

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

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.

Some common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, molecular formula is C4H6N2, 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. Formula: C4H6N2

A mixture of phosphoryl chloride (467 gm, 3.045 moles) and DMF was stirred for 1 hour at 0-5 C. The reaction is exothermic so temperature should be below 5 C. To this slowly added 1-methyl-1H-pyrazole (50 gm, 0.6090 moles) and stirred for 30 min at 0-5 C. Then slowly raised the temperature from 20-30 C. to 60-70 C. and stirred for 10-15 hours. Progress of the reaction was monitored by HPLC. The reaction mixture was cooled to 0-5 C., to this added ethyl acetate (250 ml), DM water (1 L) and aqueous ammonia solution (350 ml, pH-6 to 7). The reaction mixture was stirred for 1 hour at 20-30 C. The inorganic salt obtained was filtered off, washed with ethyl acetate (250 ml). The filtrate was transferred in to a separating funnel. The reaction mixture was allowed to settle. The organic layer was separated and aqueous layer was extracted with ethyl acetate (250 ml). The entire organic layer was transferred to the reaction vessel, stirred for 10-15 min and separated the final aqueous layer and organic layer. The combined organic layer having 1-methyl-1H-pyrazole-4-carbaldehyde and ethyl acetate was used as such for Step 2 without any purification or isolation at this step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 930-36-9, 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. 215610-30-3, name is 5-Methoxy-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H6N2O

To a solution of 3-methoxy-lH-pyrazole (520 mg, 5.3 mmol, 1 equiv) in dry THF was added NaH (60 % in mineral oil, 1.06 g, 26.5 mmol, 5 equiv) at 0C. The reaction was stirred for 1 min at room temperature under nitrogen atmosphere. Then a solution of 2- isothiocyanato-l,3-dimethoxybenzene (1.56 g, 8 mmol, 1.5 equiv) in THF (5 mL) was added. The resulting mixture was stirred at room temperature for 4 hours. The reaction was quenched with H2O (30 mL) and extracted with EtOAc (3 * 50 mL). The combined organic extracts were washed with brine (30 mL), dried over anhydrous Na2S04, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (eluted with DCM/MeOH = 100/1) to afford the title compound N-(2,6- dimethoxyphenyl)-3-methoxy-lH-pyrazole-l -carbothioamide as a white solid (l.lg, 48% yield). LC-MS: m/z 294.1 (M+H)+

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.

Related Products of 31230-17-8, A common heterocyclic compound, 31230-17-8, name is 5-Methyl-1H-pyrazol-3-amine, molecular formula is C4H7N3, 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.

PREPARATION 19; feri-Butyl 3-amino- -methyl-1 H-pyrazole-1 -car boxy late; Sodium hydride (60percent dispersion in mineral oil, 0.81 g, 33.96 mmol) was added slowly to a stirred suspension of 5-methyl-1 H-pyrazol-3-amine (3.00 g, 30.90 mmol) in tetrahydrofuran (150 mL) at 0 ¡ãC. The mixture was stirred for 30 minutes, then di-tert- butyl dicarbonate (7.40 g, 33.96 mmol) was added to the reaction. The mixture was stirred and warmed to room temperature. After 2 hours, saturated aqueous sodium hydrogencarbonate solution was added to the reaction and the mixture was extracted with chloroform. The organic layer was washed with brine, dried (Na2S04) and evaporated. Followed by purification of the crude product by flash chromatography (2.44 g, 40percent).LRMS (m/z): 198 (M+1 )+.1 H NMR (400 MHz, METHANOL-^) delta ppm 1.61 (s, 9 H) 2.10 (s, 3 H) 4.85 (s, 2 H) 5.24 (s, 1 H)

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. 69843-13-6, name is 1-Methyl-1H-pyrazol-4-amine, A new synthetic method of this compound is introduced below., name: 1-Methyl-1H-pyrazol-4-amine

Example 4.082- [ [5-Fluoro-2- [(l-methylpyrazol-4-yl)aminol -4-pyridyll amino I -N-methyl-benzamide A mixture of l-methylpyrazol-4-amine (41.7 mg, 0.43 mmol), 9,9-dimethyl-4,5- bis(diphenylphosphino)xanthene (41.4 mg, 0.07 mmol), bis(dibenzylideneacetone)palladium (32.7 mg, 0.057 mmol), sodium tert-butoxide (51.5 mg, 0.54 mmol), and 2-[(2-chloro-5-fluoropyridin-4-yl)amino]-N-methylbenzamide (100 mg, 0.36 mmol) was suspended in dioxane (3 mL). The mixture was heated at 150C for 30 minutes in a microwave reactor and then allowed to cool to room temperature. The mixture was loaded onto an SCX column and the product eluted first with MeOH and then with a 7M solution of NH3 in MeOH. Fractions containing product were combined and evaporated. The residue was purified by preparative HPLC and fractions containing product were combined and evaporated to afford example 4.08 (51.2 mg, 42% yield); 1H NMR spectrum: (300 MHz, DMSO) delta 2.78 (3H, d), 3.77 (3H, s), 6.66 – 6.68 (IH, m), 7.07 – 7.10 (IH, m), 7.31 (IH, s), 7.47 – 7.56 (2H, m), 7.69 – 7.72 (IH, m), 7.84 (IH, s), 7.91 – 7.92 (IH, m), 8.51 (IH, s), 8.64 (IH, q), 10.08 (IH, d); Mass spectrum: m/z (ESI+) (M+H)+ = 341.04.

The synthetic route of 69843-13-6 has been constantly updated, and we look forward to future research findings.

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. 288-13-1, name is 1H-Pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Safety of 1H-Pyrazole

A solution of lH-pyrazole (30 g, 440 mmol) in tetrahydrofuran (500 mL) was treated with sodium hydride (26 g, 648 mmol, 60%) at 0 C, and then stirred for 1 h at 0 C. N,N-Dimethylsulfamoyl chloride (95 g, 661 mmol) was added dropwise at 0 C. The resulting solution was stirred for additional 2 h at room temperature and then quenched by water. The resulting solution was extracted with dichloromethane and concentrated in vacuo. The residue was purified by flash chromatography on silica gel eluting with ethyl acetate/petroleum ether (1/6) to afford to N,N-dimethyl-lH-pyrazole-l -sulfonamide ( 58 g, 75%) as colorless oil. LCMS (ESI): M+H+ = 175.0.

The synthetic route of 288-13-1 has been constantly updated, and we look forward to future research findings.

1904-31-0, name is 1-Methyl-1H-pyrazol-3-amine, 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. Recommanded Product: 1904-31-0

4-Chloro-6-[(1-methyl-1H-pyrazol-3-yl)amino]-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile 4,6-Dichloro-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile (0.118 g), 1-methyl-1H-pyrazol-3-amine (0.027 g), sodium tert-butoxide (0.269 g), tris(dibenzylideneacetone)dipalladium(0) (0.026 g) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos, 0.035 g) were added to a microwave vial, followed by dry DMF (5 mL). The reaction mixture was flushed with N2 for ?10 min, and then heated to 80¡ã C. with microwaves for 1 h. The reaction mixture was subjected to silica-gel flash column chromatography [dichloromethane-methanol (2-3percent)]. The eluted material, obtained as a yellow solid (0.055 g, 78percent) was identified as 4-chloro-6-[(1-methyl-1H-pyrazol-3-yl)amino]-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile. LC-MS (Method A) (m/z) 273 (M+H+); tR=2.11.

The synthetic route of 1904-31-0 has been constantly updated, and we look forward to future research findings.

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. 67-51-6, name is 3,5-Dimethyl-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Product Details of 67-51-6

3,5-Dimethyl-1H-pyrazole, 78.5 g (0.818 mol), was dissolved in 700 mL of water heated to 70C, and 517 g (3.271 mol) of potassium permanganate was added to the hot solution, maintaining the temperature no higher than 90C. The mixture was cooled to room temperature, the precipitate of MnO2 was filtered off and washed with water, and the filtrate was acidified with aqueous HCl to pH 2 and left overnight. The precipitate was filtered off and washed with water. Yield 41.75 g (33%), white crystals, mp 257-258C. 1H NMR spectrum: delta 7.07 ppm, s (1H, 4-H). 5-Methyl-1H-pyrazole-3-carboxylic acid (2). The aqueous filtrate obtained after separation of diacid 1, was neutralized to pH 5-6, and the precipitate of 2 was filtered off and washed with water. Yield 18.1 g (18%), white crystals, mp 210-211C. 1H NMR spectrum, delta, ppm: 2.25 s (3H, CH3), 6.42 s (1H, 4-H).

The synthetic route of 67-51-6 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, 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. SDS of cas: 930-36-9

Adding 5.92 g (20 mmol) of FeBr3 to a solution of 8.2 g (100 mmol) of 1-methylpyrazole dissolved in 100 mL of methyl tert-butyl ether at 0 ;Under stirring, 32 g (200 mmol) of Br2 was added dropwise.Stir at room temperature,The end of the reaction was followed by TLC.After confirming the reaction,Filter the system,The filtrate is poured into the water.Use Na2S2O3 solution in sequence,Water washing,Liquid separation.The obtained organic phase was dried over anhydrous magnesium sulfate.The solvent was evaporated under reduced pressure,Got 14.5g(yield: 90.5%, purity 98%)5-bromo-1-methylpyrazole.

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