Month: April 2021

Reference of 2644-93-1, These common heterocyclic compound, 2644-93-1, name is 1,3,5-Trimethyl-1H-pyrazole-4-carbaldehyde, 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.

At room temperature for 6-bromo-4-chloro-2-methoxy-3 – (4 – (trifluoromethyl) benzyl) quinoline (1.37 g, 3.86 mmol, Intermediate 10: step d) comprises that the flask, THF It was added (45 mL) to obtain a colorless, homogeneous mixture.Cooling the solution to -78 Next,ndropwise -BuLi (2.5 M, 1.8 mL, 4.5 mmol in hexane).The color of the solution was reddish brown.4 minutes after, 1,3,5-trimethyl -1H-pyrazole-4-carbaldehyde (300 mg, 2.17 mmol, 3 mL of THF) was introduced to he a mixture of red-brown color over 5 min It was in turn greenish yellow.The mixture was warmed to 0 over 45 minutes and, at this time the reaction NH4was quenched with aqueous solution of Cl.The mixture was diluted further with water and extracted with EtOAc (3 ¡Á 150 mL).The combined organics were washed with brine, MgSO4dried, filtered, and concentrated to give a light orange foam.Silica gel by FCC on (2% MeOH-DCM, increased to 8% MeOH-DCM), to give the title compound as a pale yellow non-crystalline solid.

The synthetic route of 2644-93-1 has been constantly updated, and we look forward to future research findings.

Related Products of 110860-60-1, 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. 110860-60-1, name is Methyl 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.

(5) Synthesis of alpha-Type Crystal Morphology Azo Pigment Compound (2) (9.2 g) was dissolved in a mixed solution of 55 mL of acetic acid and 37 mL of propionic acid at room temperature, and the resulting solution was ice-cooled to lower the internal temperature to -3 C. A 40 mass % sulfuric acid solution of nitrosylsulfuric acid was added dropwise at an internal temperature of -3 C. to 4 C. over 10 minutes and after stirring at an internal temperature of 4 C. for 1 hour, 0.2 g of urea was added. Thereafter, the internal temperature was lowered to -3 C., and the mixture was further stirred for 10 minutes to obtain a diazonium salt solution. Separately, 10 g of Compound (3) was completely dissolved in 150 mL of acetone. This solution was cooled to an internal temperature of 17 C. and then added to the diazonium salt solution obtained above, at an internal temperature of -3 C. to 3 C. over 25 minutes. After the completion of addition, the mixture was stirred at 3 C. for 30 minutes, and the ice bath was removed. The temperature was raised to room temperature over 30 minutes, and the resulting solution was stirred at room temperature for 30 minutes. The obtained crystal was collected by filtration, spray-washed with 150 mL of acetone and further spray-washed with 100 mL of water. The obtained crystal was without drying suspended in 400 mL of water, and an aqueous 8 N potassium hydroxide solution was added to adjust the pH to 5.7. The system was stirred at room temperature for 20 minutes, and the obtained crystal was separated by filtration, thoroughly spray-washed with water and spray-washed with 80 mL of acetone. The obtained crystal was dried at room temperature for 12 hours.Crystal 1 obtained was suspended in 580 mL of acetone, and the suspension was stirred under reflux for 30 minutes and then cooled to room temperature over 10 minutes. The obtained crystal was separated by filtration and dried at 60 C. for 5 hours to obtain 17.1 g of an azo pigment composition containing an azo pigment represented by formula (1) having the crystal form of the present invention. Yield: 88.5%. The particle size of the obtained azo pigment was measured with an eye by using a transmission microscope (electron microscope JEM-1010, manufactured by JEOL Ltd.), as a result, the length in the long axis direction of the primary particle was about 15 mum.The obtained crystal was an alpha-type crystal morphology azo pigment shown in FIG. 1 or a tautomer thereof, having characteristic X-ray diffraction peaks at Bragg angles (2theta+/-0.2) of 7.6, 25.6 and 27.7 in the CuKalpha characteristic X-ray diffraction but not having a peak at 7.0 and 6.4 (alpha-Type Crystal Morphology Azo Pigment Composition 1).

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

Adding a certain compound to certain chemical reactions, such as: 852443-61-9, name is 3-(Trifluoromethyl)-1H-pyrazol-5-amine, 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 852443-61-9, HPLC of Formula: C4H4F3N3

-((2-Chloro-4-fluorobenzyl)carbamothioyl)-3,4-difluorobenzamide (98.0 g, 273 mmol) and 5-amino-3-trifluoromethylpyrazole (41.3 g, 273 mmol) were dissolved in THF (546 mL). Nl-((Ethylimino)methylene)-N3,N3-dimethylpropane-l,3-diamine hydrochloride (57.6 g, 300 mmol) was added and the reaction was stirred at room temperature for 1 h and then heated to 40 C for 15 h. The crude mixture was diluted with water (500 mL) and isopropyl acetate (500 mL). The organic layer was washed with brine (500 mL), dried over sodium sulfate, and concentrated. The residue was diluted with isopropyl acetate (1.3 L) and heated to 65 C for 1 hour. The solution was allowed to cool to room temperature, filtered and the filtrate was concentrated. The residue was heated to70C in acetonitrile (900 mL) and then allowed to cool to room temperature. The resulting suspension was filtered, rinsed with acetonitrile (200 mL) and dried in vacuo at 60C to afford 55 g (43%) of (Z)-N-(((2-chloro-4- fluorobenzyl)amino)((3-(trifluoromethyl)-lH-pyrazol-5-yl)amino)methylene)-3,4- difluorobenzamide as a white solid. 1HNMR (400 MHz, MeOH-d4) delta 7.95 (bs, 2H), 7.50 (t, 1H, J=7.2Hz), 7.26 (m, 2H), 7.06 (t, 1H, J=7.5 Hz), 6.56 (s, 1H), 4.84 (s, 2H).

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

Synthetic Route of 10010-93-2, A common heterocyclic compound, 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole, molecular formula is C5H5F3N2, 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.

[00143] Step 1: A mixture of 2-chloro-l-(l-(4-chloro-3-methoxyphenyl)piperidin- 4-yl)ethanone (580 mg, 1.919 mmol; see Example Ia, Step 2), 5-methyl-3- (trifluoromethyl)-lH-pyrazole (576 mg, 3.84 mmol), potassium carbonate (796 mg, 5.76 mmol) and acetonitrile (20 mL) was stirred at RT for 12 h. After this time, the solvent was removed under reduced pressure and the resultant residue was partitioned between EtOAc (10OmL) and water (50 mL). The organic phase was washed with brine, dried (TS^SO4) and concentrated on a rotary evaporator to yield a residue. The residue was purified by flash chromatography using a 40 g silica gel cartridge and gradient elution from 10: 1 Hex/EtOAc to 1 : 1 Hex/EtOAc. The fractions containing the product were pooled and concentrated on a rotary evaporator to give l-(l-(4- chloro-3-methoxyphenyl)piperidin-4-yl)-2-(5-methyl-3-(trifluoromethyl)-lH-pyrazol- l-yl)ethanone (650 mg, 1.563 mmol, 81 % yield) as clear oil. 1H-NMR (400 MHz, CDCl3) delta ppm 7.19 (1 H, d, J=8.57 Hz), 6.49 (1 H, d, J=2.42 Hz), 6.44 (1 H, dd, J=8.68, 2.53 Hz), 6.35 (1 H, s), 5.01 – 5.04 (2 H, m), 3.84 – 3.89 (3 H, m), 3.62 – 3.69 (2 H, m), 2.77 (2 H, td, J=12.03, 2.75 Hz), 2.58 (1 H, tt, J=I 1.29, 3.87 Hz), 2.21 (3 H, s), 1.99 (2 H, s), 1.80 – 1.91 (2 H, m).

The synthetic route of 10010-93-2 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. 70951-85-8, name is 4-Bromo-1-(tert-butyl)-1H-pyrazole, A new synthetic method of this compound is introduced below., Safety of 4-Bromo-1-(tert-butyl)-1H-pyrazole

A solution of 4-bromo-1-tert-butyl-1H-pyrazole (973 mg, 4.79 mmol) in anhydrous THF (9.5 ml) was cooled to -78 C. under argon. A solution of n-BuLi in Hexanes (1.6 M, 3.2 mL, 5.12 mmol) was then added dropwise over 5 min and reaction mixture was stirred at -78 C. for 80 min. A solution of N-methoxy-N-methylacetamide (0.55 ml, 5.17 mmol) in THF (3 mL) was added dropwise and mixture was warmed to 0 C. After 4 hours, reaction mixture was quenched via addition of NH4Cl (aq) (10 mL) and mixture was extracted with ethyl acetate. Combined organic layers were washed with 50% brine, dried (Na2SO4), filtered, and concentrated under reduced pressure. Resulting residue was purified by silica gel column chromatography (0-50% ethyl acetate in hexanes) to yield 1-(1-tert-butyl-1H-pyrazol-4-yl)ethanone 5.14.

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.

Some common heterocyclic compound, 138786-86-4, name is Methyl 4-nitro-1H-pyrazole-3-carboxylate, molecular formula is C5H5N3O4, 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. Product Details of 138786-86-4

A mixture of sodium hydride (167 mg, 6. [96] mmol) in tetrahydrofuran (15 mL) cooled to [0 oC] was treated with a solution [OF 4-NITRO-LH-PYRAZOLE-3-CARBOXYLIC] acid methyl ester (1.0 g, 5.8 mmol) in tetrahydrofuran (10 mL). This mixture was stirred at [0 oC] for 1 h. It was then treated with methyl iodide (0.54 mL, 8.7 mmol). The reaction was stirred at [25 oC] for 18 h. At this time, the reaction was cooled to 0 oC and was then quenched with a saturated aqueous ammonium chloride solution and diluted with ethyl acetate (200 mL). This solution was washed with water (1 x 100 mL) and a saturated aqueous sodium chloride solution (1 x 100 mL). The organics were dried over magnesium sulfate, filtered, and concentrated in vacuo. The resulting solid was slurried in 40% ethyl acetate/petroleum ether and cooled in the freezer for 15 min. At this time, the solids were collected by filtration to afford [L-METHYL-4-NITRO-LH-] pyrazole-3-carboxylic acid methyl ester (889 mg, 82.8%) as a white solid

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 138786-86-4, 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. 25699-98-3, name is 4′-(1-Pyrazolyl)acetophenone, A new synthetic method of this compound is introduced below., name: 4′-(1-Pyrazolyl)acetophenone

General procedure: To a 15 mL dry Schlenk tube with a stirring bar, substrate 1 (0.3 mmol), 2 (0.36 mmol), and [Cp*Co(CO)I2] (5 mol%) were added under air. Then the tube was transferred into the glove box. AgSbF6 (10 mol%) was added. After moving out, DCE(2 mL) was injected into the tube under nitrogen. Then the tube was sealed and the mixture was stirred at 100 C for 12-48 hours. After cooling down, the solvents were removed under reduced pressure and the residue was purified by column chromatography on silica gel (petroleum ether/ethyl acetate) to give the desired coupling product.

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 118430-74-3,Some common heterocyclic compound, 118430-74-3, name is 3-Cyclopropyl-1-methyl-1H-pyrazol-5-amine, molecular formula is C7H11N3, 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.

A mixture of 3-cyclopropyl-1-methyl-1H-pyrazol-5-amine (3 g, 22 mmol, Fluorochem), 4-chloro-2-methylbenzaldehyde (3.1 g, 22 mmol, Fluorochem), and 2-mercapto-2-methylpropanoic acid (3.5 g, 33 mmol, Chemwish) was heated, in a sealed microwave vessel, for about 60 min, at about 80 C. Subsequently, the reaction mixture was heated, for about 24 h, at about 150 C. After cooling to rt, acetonitrile (20 mL) was added and the reaction mixture was stirred for about 2 h, at about 40 C. After cooling to about 0 C., the precipitated solid was collected by filtration and washed with acetonitrile (2 mL) to afford 4-(4-chloro-2-methyl-phenyl)-3-cyclopropyl-1,6,6-trimethyl-4,8-dihydropyrazolo[3,4-e][1,4]thiazepin-7-one as white solid (1.25 g, 3.3 mmol, 15%). 1H-NMR (CDCl3, Bruker 400 MHz) delta 0.30-0.39 (1H, s); 0.46-0.67 (3H, m); 0.83-0.93 (1H, m); 1.50 (3H, s); 1.66 (3H, s); 2.48 (3H, s); 3.75 (3H, s); 5.58 (1H, s); 7.09 (1H, dd, J=8.5, 2.5 Hz); 7.14 (1H, d, J=2.5 Hz); 7.21 (1H, d, J=8.5 Hz); H, m); 8.65 (1H, s).

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

Application of 1203705-55-8, The chemical industry reduces the impact on the environment during synthesis 1203705-55-8, name is 3-Bromo-1H-pyrazol-5-amine, I believe this compound will play a more active role in future production and life.

To a solution of 3-bromo-1H-pyrazol-5-amine (3.2 g, 20.0 mmol) in DMF (60 mL) were added Cs 2CO 3 (13.0 g, 40.0 mmol) and ethyl-3-ethoxyacrylate (8.6 g, 60.0 mmol), the reaction mixture was stirred at 125 C for about 2 h. The reaction mixture was cooled to ambient temperature, poured into H 2O (200 mL), acidified by 1N HCl acid solution, extracted with EA (100 mL 3). The combined organic layers were washed with H 2O (100 mL), concentrated and purified by chromatography on silica gel (eluent: DCM/MeOH = 10/1) to afford the desired compound as a yellow solid (2.0 g). MS (ESI, m/e) [M+1] + 213.9, 214.9.

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

31037-02-2, name is Ethyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, 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. Product Details of 31037-02-2

Example 19A Ethyl 5-butylamino-1-methylpyrazole-4-carboxylate To ethyl 5-amino-1-methylpyrazole-4-carboxylate (3.4476 g, 20.38 mmol) in dimethylformamide (60 mL) at 0 C. was added a solution of 1.0M sodium bis(trimethylsilyl)amide in tetrahydrofuran (20.5 mL, 20.5 mmol). After 1 hour, 1-iodobutane (2.50 mL, 22.0 mmol) was added and the reaction was stirred at ambient temperature for 20 hours. The mixture was diluted with saturated aqueous sodium bicarbonate and extracted with ethyl acetate (6*). The combined organic extracts were then washed with water (2*) and brine, dried over sodium sulfate, filtered and evaporated under reduced pressure. Chromatography of the residue on silica gel eluding with 20% ethyl acetate in hexane afforded 3.8754 g (84%) of the desired product as a oil. TLC (20% ethyl acetate/80% hexane) Rf =0.12. 1 H NMR (CDCl3, 300 MHz) d 0.94 (t, 3H), 1.33 (t, 3H), 1.35-1.50 (m, 2 H), 1.53-1.65 (m, 2H), 3.25 (t, 2H), 3.77 (s, 3H), 4.25 (q, 2H), 5.60-5.80 (br, 1H), 7.62 (s, 1H). MS (DCl/NH3)m/e 226 (M+H)+.

The synthetic route of 31037-02-2 has been constantly updated, and we look forward to future research findings.