Month: April 2021

Electric Literature of 20154-03-4,Some common heterocyclic compound, 20154-03-4, name is 3-(Trifluoromethyl)-1H-pyrazole, molecular formula is C4H3F3N2, 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: The considered 3-trifluoromethylpyrazole (68 mmol) was dissolved in 50percent aqueous sulfuric acid (20 mL). This was cooled to 0 ¡ãC and N-iodosuccinimide (18.5 g, 82 mmol) was added. The suspension was stirred 10 min at 0 ¡ãC and then stirred, 3 h for 1e and two days for 1f, at room temperature. This was dispersed in water (500 mL) and stirred overnight. The precipitate was filtered, washed with water and redispersed in boiling water (400 mL), a small amount of sodium disulfite was added and the suspension was left to cool, filtered again and dried under vacuum to yield compound 2e or 2f as described below.

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

Electric Literature of 2075-46-9, 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. 2075-46-9, name is 4-Nitro-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a stirred solution of 4-nitro-1H-pyrazole (2 g, 17.7 mmol) inacetonitrile (15 mL) was added potassium carbonate (2.7 g, 19.5 mmol)and iodomethane (2.76 g, 19.5 mmol). The reaction mixture was stirredat reflux temperature for 6 h. And it was evaporated to dryness. Thecrude mass was purified by silica gel column chromatography (PE:EA=10:1) to afford compound 15c (2.2 g, 98%) as a white solid. MS(ESI) m/z 128 [M+H]+.

The synthetic route of 4-Nitro-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Application of 10250-63-2, 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. 10250-63-2, name is Ethyl 1-methyl-3-phenyl-1H-pyrazole-5-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Production Example 197c) 0.12 g of ethyl 1-methyl-3-phenyl-1H-5-pyrazolecarboxylate was dissolved in 5 ml ethanol. 1 ml of 5N aqueous sodium hydroxide solution was added thereto, followed by heating under reflux for 1 hour. The reaction solution was ice-cooled, neutralized with 2N hydrochloric acid and then extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and evaporated, to give 0.11 g of 1-methyl-3-phenyl-1H-5-pyrazolecarboxylic acid. 1H-NMR(CDCl3) delta: 4.22(s, 3H) 7.22(s, 1H) 7.33(t, J=8.0Hz, 1H) 7.40(t, J=8.0Hz, 2H) 8.80(d, J=8.0Hz, 2H)

The synthetic route of Ethyl 1-methyl-3-phenyl-1H-pyrazole-5-carboxylate 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. 4522-35-4, name is 3-Iodo-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. category: pyrazoles-derivatives

INTERMEDIATE 6 3-Iodo-l-(4-(methylsulfonyl)phenyl)-lH-pyrazole To a solution of 3-iodopyrazole (0.7 g, 3.61 mmol) in DMSO (18.0 mL) was added sodium hydride (60% disp. in oil, 0.173 g, 4.33 mmol) and the resulting mixture was stirred for 0.5 h before adding 4-methylsulfoylfluorobenzene (0.629 g, 3.61 mmol). The reaction mixture was stirred at 90 C for 3 h. The reaction was quenched by the addition of water and extracted with EtOAc. The combined organic extracts were washed with water and brine, dried over MgS04 and concentrated in vacuo. The crude mixture was purified by flas chromatography (ISCO, 40 g, 0-60 % EtOAc in hexanes) to afford 3-iodo-l-(4-(methylsulfonyl)phenyl)-lH-pyrazole, as a white solid. LCMS calc. = 348.94; found = 348.92 (M+H)+. 1H NMR (500 MHz, CDC13): delta 8.03 (dd, J= 8.7, 1.7 Hz, 2 H); 7.89 (dd, J= 8.7, 1.7 Hz, 2 H); 7.84 (d, J= 2.6 Hz, 1 H); 6.69 (d, J= 2.6 Hz, 1 H); 3.09 (s, 3 H).

The synthetic route of 4522-35-4 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 2075-46-9, A common heterocyclic compound, 2075-46-9, name is 4-Nitro-1H-pyrazole, molecular formula is C3H3N3O2, 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.

[0223j To a mixture of 4-nitro-1H-pyrazole (113 mg, 1 mmol, 1.0 eq) in CH3CN (5 mL), 1-bromo-2-methoxyethane (138 mg, 1 mmol, 1.0 equiv) and K2C03 (276 mg, 2 mmol, 2.0 equiv) was added. The mixture was stirred at 80 C for 4 h. After diluted with EtOAc (100 mL), the mixture was washed with water (50 mL x 2). The organic layer was concentrated and purified by silica gel column (petroleum ether/EtOAc = 10 : 1) to give 1-(2-methoxyethyl)-4-nitro-1H- pyrazole (170 mg, yield: 100%) as a colorless oil. ESI-MS (M+H): 172.1. ?H NMR (400 MHz, CDC13) (5: 8.23 (s, 1H), 8.07 (s, 1H), 4.31 (t, J= 5.2 Hz, 2H), 3.74 (t, J= 5.2 Hz, 2H), 3.35 (s, 3H).

The synthetic route of 2075-46-9 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. 2075-46-9, name is 4-Nitro-1H-pyrazole, A new synthetic method of this compound is introduced below., Safety of 4-Nitro-1H-pyrazole

At 0 C,Concentrated sulfuric acid (50 ml)Was slowly added to the pyrazole (14 g)Concentrated nitric acid (9.2 ml) was then slowly added to the mixture, and the reaction was stirred at 60 C for 1.5 hours.After completion of the reaction, the reaction solution was slowly added to an appropriate amount of ice water, and the resulting white solid was separated by filtration, and the resulting solid was allowed to dry in air,The filtrate was extracted with ethyl acetate (30 ml x 3)The organic phase liquid was then rotary evaporated and dried, and finally the two parts of the solid were combined to give the compound 1a,1a (6 mmol) was dissolved in dry DMF (6 ml)Then, K2CO3 (9 mmol), methyl iodide (12 mmol),The reaction was stirred at room temperature for 16 hours.After completion of the reaction, the reaction solution was extracted with water and ethyl acetate (25 ml x 3)The organic phase was then removed with anhydrous magnesium sulfate.Finally, the organic phase was evaporated under vacuum to dryness to give a crude product,And purified by silica gel column chromatography to obtain Compound 2a.Compound 2a (2 mmol) was dissolved in absolute ethanol (5 ml)Then, palladium carbon (0.04 g) was added successively thereto,Hydrazine hydrate (1 ml), and the reaction solution was stirred at 80 C for 10 minutes.After completion of the reaction, the reaction solution was filtered to remove palladium carbon, and the filtrate was evaporated to dryness under reduced pressure in vacuo to give Compound 3a.Bromoacetic acid (2 mmol) was dissolved in dichloromethane (15 ml), and HOBt (2 mmol) was added thereto successively,EDC (2 mmol), and the reaction solution was stirred at room temperature for 30 minutes,The resulting 3a was then added and the reaction was stirred at room temperature for 12 hours.After completion of the reaction, the reaction solution was extracted with water and dichloromethane (30 ml x 3)Finally, the organic phase liquid was evaporated to dryness and the resulting crude product was purified by silica gel column chromatography to obtain Compound 4a.The resulting compound 4a, indole (2 mmol), NaH (2.4 mmol) was added to dry DMF (10 mL)The reaction solution was stirred at room temperature for 12 hours, and then quenched by adding saturated brine to the reaction.The resulting reaction mixture was extracted with saturated brine and ethyl acetate (30 mL x 3)The organic phase was then removed with anhydrous magnesium sulfate.Finally, the organic phase was evaporated under vacuum to dryness to give a crude product,And purified by silica gel column chromatography to obtain the final compound 5a to give a red solid powder in a yield of 60%

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.

Application of 68703-67-3, 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. 68703-67-3 name is 4-Amino-1H-pyrazole-3-carbonitrile, 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.

In 500mLIn the eggplant-shaped bottle, add 125mL of distilled water and 50mL of DCM,Add with full agitationSulfur phosgene (2.04mL, 26mmol),Compound 4 (2.63g, 24mmol) was dissolved in 75mL DCM and slowly added to the reaction solution, and stirred at room temperature for 1h after the addition.After the reaction was completed, it was allowed to stand for separation, and the organic phase was successively distilled water.Wash three times with saturated brine, dry with anhydrous sodium sulfate, and filter with suction.The filtrate was concentrated under reduced pressure to obtain 1.78 g of a yellow solid with a yield of 48%. TLC (PE: EA = 2: 1, v / v).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Amino-1H-pyrazole-3-carbonitrile, and friends who are interested can also refer to it.

Synthetic Route of 31108-57-3, A common heterocyclic compound, 31108-57-3, name is 1H-Pyrazole-4-carbonitrile, molecular formula is C4H3N3, 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 mixture of ABl (100 mg, 0.235 mmol) and K2C03 (64.9 mg, 0.47 mmol) in acetone (5 mL) was added lH-pyrazole-4-carbonitrile (32.7 mg, 0.352 mmol) at 25C. The reaction mixture was stirred at the 25C for 16 h. Then saturated aqueous H20 (50 mL) was added .The mixture was extracted with EtOAc (3 x 50 mL). The combined organic solution was washed with brine (20 mL), dried over Na2S04 and concentrated in vacuum to give the crude product .The crude product was purified by flash column (0-30% of EtOAc in PE) to give Compound 66 (38 mg, 37%) as a solid. (0895) 1H NMR (400 MHz, CDC13) delta 7.86 (s, 1H), 7.81 (s, 1H), 5.00 (d, J = 16.0 Hz, 1H), 4.85 (d, J = 16.0 Hz, 1H), 2.71-2.68 (m, 1H), 2.18-2.09 (m, 1H), 1.98-1.96 (m, 1H), 1.65-1.53 (m, 2H), 1.52-1.50 (m, 5H), 1.37-1.14 (m, 14H), 0.97 (d, J= 8 Hz, 4H), 0.85-0.81 (m, 1H), 0.75 (s, 3H), 0.68 (s, 3H). (0896) LCMS Rt = 2.594 min in 4.0 min chromatography, 30-90AB_220&254.1cm, purity 100%, MS ESI calcd. for C27H38N3O [M+H-H20]+ 420, found 420.

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.

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 31230-17-8 as follows. SDS of cas: 31230-17-8

A mixture of 2,4-dichloropyrimidine (0.967 g, 6.49 mmol), 3-amino-5-methylpyrazole (0.63 g, 6.40 mmol), and ethyldiisopropylamine (2.8 mL, 16.22 mmol) in ethanol (13 mL) was stirred at -10C for 2 h, then at r.t. overnight, and finally at 50C for 3.5 h. The mixture was concentrated to a total volume of approximately 10 mL. Upon repeated addition of diethylether, (2-chloropyrimidin-4-yl)-(5-methylpyrazol-3-yl)amine (0.258 g, 1.23 mmol, 19 %) was obtained as colourless crystals. LC/ESI-MS: m/z = 210 [M(35Cl) +H]+; m/z = 208 [M(35Cl)-H]-; Rt = 2.30 min.

According to the analysis of related databases, 31230-17-8, the application of this compound in the production field has become more and more popular.

Reference of 1572-10-7,Some common heterocyclic compound, 1572-10-7, name is 3-Amino-5-phenylpyrazole, molecular formula is C9H9N3, 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: The general method was described for the synthesis of D1. Compound C1 (150 mg, 0.393 mmol) was dissolved in ethanol (2 mL),followed by addition of 5-phenyl-1H-pyrazol-3-amine (62.63 mg, 0.393 mmol) and triethylamine (119.43 mg, 1.18 mmol). The mixture was stirred at room temperature for 5 h. The resultant mixture was purified by column chromatography to give D1.

The synthetic route of 1572-10-7 has been constantly updated, and we look forward to future research findings.