Month: May 2021

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. 15802-80-9, name is 3-(tert-Butyl)pyrazole, This compound has unique chemical properties. The synthetic route is as follows., Safety of 3-(tert-Butyl)pyrazole

Reference Example 274 To a mixture of3-tert-butyl-lH-pyrazole (3.72 g), 2-chloro-5- (trifluoromethyl) pyridine (5.45 g) and N- methylpyrrolidone (18.6 ml) was added sodium hydroxide (1.80 g) while stirring the mixture at room temperature. After allowing reaction as it was for 8 hours, water (38 ml) and 6N hydrochloric acid (80 ml) were added and the mixture was extracted with ethyl acetate. The extract was washed with water and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography, and eluted with hexane and then with toluene to give2- (3-tert-butyl-lH-pyrazol-1-yl)-5-(trifluoromethyl) pyridine (7.04 g, yield87%) as a colorless oil. H-NMR (CDC13) 5 : 1.37 (9H, s), 6.37 (lH, d, J=2.6 Hz), 7.97 (1H, dd, J=8.7, 2.1 Hz), 8.08 (1H, d, J=8.7 Hz), 8.46 (1H, d, J=2.7 Hz), 8.6-8. 7 (1H, m).

According to the analysis of related databases, 15802-80-9, the application of this compound in the production field has become more and more popular.

Electric Literature of 15115-52-3, 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. 15115-52-3 name is 4-Bromo-1-phenyl-1H-pyrazole, 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.

To a solution of compound 4-bromo-l -phenyl- lH-pyrazo Ie (0.5 g, 2.3 mmol) in DMSO (50 mL) was added KOAc (0.66 g, 6.8 mmol), bis(pinacolato)diboron (0.63 g, 2.5 mmol) and ¥dCb(dpp{) (0.076g, 0.11 mmol) at room temperature. The reaction mixture was stirred overnight at 8O0C. The result mixture was diluted with EA, washed with brine, dried over Na2SO4, concentrated, purified by chromatography (EA:PE=1: 12) to give l-phenyl-4-(4,4,5,5-tetramethyl-l,3,2- dioxaborolan-2-yl)-lH- pyrazole (0.3 g, 50%) as light yellow solid

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

Synthetic Route of 5744-80-9, A common heterocyclic compound, 5744-80-9, name is 3-Bromo-1,5-dimethyl-1H-pyrazole, molecular formula is C5H7BrN2, 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.

General procedure: A mixture of 19d (0.20 g, 0.81 mmol), bis(pinacolato)-diboron(0.44 g, 1.72 mmol), Pd(Ph3P)4 (0.050 g, 0.043 mmol), and KOAc (0.17 g, 1.72 mmol) in 1,4-dioxane/H2O (30 mL, v/v, 5/1) was stirred at 100 C for 4 h under argon. It was cooled to room temperature. 10a(0.20 g, 0.54 mmol), Pd(Ph3P)4 (0.030 g, 0.029 mmol), and K2CO3(0.16 g, 1.14 mmol) were added to the reaction mixture at room temperature,and the mixture was stirred at 100 C for 12 h under argon. It was cooled to room temperature, and H2O was added to the mixture.The mixture was extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silicagel column chromatography (eluting with 0-10% MeOH in DCM) to afford 10c as a pale yellow solid (0.13 g, 52%). 1H NMR (300 MHz,DMSO-d6) delta 8.27 (s, 1H), 7.78-7.75 (m, 1H), 7.54 (s, 1H), 7.18-7.15(m, 1H), 6.88-6.87 (m, 1H), 6.15 (s, 1H), 6.02-5.93 (m, 1H), 5.82-5.76(m, 1H), 5.32-5.27 (m, 1H), 5.03 (s, 2H), 3.93 (s, 3H), 3.64 (m, 4H),3.33 (m, 4H); 13C NMR (75 MHz, DMSO-d6) delta 161.85, 158.29, 156.01,153.75, 152.72, 142.91, 140.24, 139.17, 138.42, 137.18, 131.81,128.07, 126.97, 126.44, 124.53, 119.49, 116.23, 97.23, 65.97, 60.28,51.65, 41.76; MS (ESI) m/z:460.3 [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.

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. 78208-72-7, name is Ethyl 3-isopropyl-1H-pyrazole-5-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. SDS of cas: 78208-72-7

A mixture of ethyl 5-isopropyl-1H-pyrazole-3-carboxylate (Chem. and Pharm. Bull. 1984; 32(4);1568) (509 mg, 2.8 mmol), 2-(2-bromoethoxy)tetrahydro-2-pyran (732 mg, 3.5 mmol) and potassium carbonate (483 mg, 3.5 mmol) in 1-methyl-2-pyrrolidinone (5 ml) was stirred at 80° C. for 18 hours. The cooled mixture was poured into ethyl acetate and washed with water and brine, then dried (MgSO4) and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel using an elution gradient of ethyl acetate:pentane (20:80 to 40:60) to afford the title compound of preparation 34 as a clear oil, 663 mg. [0469] 1HNMR (CDCl3, 400 MHz) delta: 1.25 (d, 6H), 1.37 (t, 3H), 1.44-1.71 (m, 6H), 2.97 (m, 1H), 3.42 (m, 1H), 3.54 (m, 1H), 3.75 (m, 1H), 4.00 (m, 1H), 4.32 (q, 2H), 4.54 (t, 1H), 4.68 (m, 1H), 4.76 (m, 1H), 6.64 (s, 1H). [0470] LRMS: m/z ACPI+ 311 [MH]+ [0471] Further elution provided the title compound of preparation 35, 242 mg. [0472] 1HNMR (CDCl3, 400 MHz) delta: 1.25 (d, 6H), 1.38 (t, 3H), 1.46-1.72 (m, 6H), 3.15 (m, 1H), 3.45 (m, 1H), 3.65 (m, 1H), 3.81 (m, 1H), 4.10 (m, 1H), 4.34 (m, 2H), 4.39 (m, 2H), 4.49 (t, 1H), 6.57 (s, 1H). [0473] LRMS: m/z ACPI+ 311 [MH]+

The synthetic route of 78208-72-7 has been constantly updated, and we look forward to future research findings.

Application of 2075-45-8, A common heterocyclic compound, 2075-45-8, name is 4-Bromo-1H-pyrazole, molecular formula is C3H3BrN2, 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.

Step 1: Preparation of tert-butyl 4-bromo-lH-pyrazole-l-carboxylate B [00161] Boc anhydride (2.34 niL, 10.2 mmol) was added to a solution of 4-bromo-lH- pyrazole (1 g, 6.8 mmol), triethylamine (3.3 raL, 23.8 mmol) and 4-dimethylaminopyridine (0.166 g, 1.36 mmol) in acetonitrile (20 mL) at 0 C and the reaction mixture was stirred at room temperature for 2 h. The reaction mixture was diluted with water and extracted with ethyl acetate (100 niL x 3). The combined organic extract was washed with water (100 mL), brine (100 raL), dried over anhydrous sodium sulfate and evaporated. The crude material was purified by combiflash purifier using 10% ethyl acetate in hexane to afford the title compound tert-butyl 4- bromo-1 H-pyrazole- 1 -carboxylate (1.65 g, 98% yield) as a colorless liquid. FontWeight=”Bold” FontSize=”10″ H NMR (400 MHz, CDCls) delta 8.09 (s, 1H), 7.66 (s, 1H), 1.65 (s, 9H).

The synthetic route of 2075-45-8 has been constantly updated, and we look forward to future research findings.

3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, 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. Formula: C4H5N3O2

General procedure: To 17a (1 g, 7.8 mmol) in EtOH (20 mL) was added 10% Pd/C50 mg. The reaction mixture was stirred for 3 h under hydrogen at roomtemperature. The mixture was then filtered with Celite, and the filtratewas concentrated and dried under vacuum to yield 0.74 g (97%) of 18aas a white solid. MS (ESI) m/z 98 [M+H]+.

The synthetic route of 3994-50-1 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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: 1280210-79-8

Under N2 protection and a condition free of water and oxygen, Intermediate 2 (1000 mg, 4.78 mmol) was dissolved in N,N-dimethylformamide (15 ml), which was cooled to -15C, and sodium bis(trimethylsilyl)amide (4.78 mL, 2 mol/L, 9.56 mmol) was added, followed by stirring for 30 min, and S-tetrahydrofuran-3-ylsulfonyl chloride (1.39 g, 8.13 mmol) was added dropwise to the reaction solution, followed by reaction for 16 hours at this temperature. The temperature was raised to 0C, and the reaction was quenched by addition of water (20 ml) to the reaction solution, which was then extracted with ethyl acetate (20 ml*2). The organic phases were combined, dried over anhydrous sodium sulfate, concentrated, re-dissolved in tetrahydrofuran (20 ml), and cooled to -10C to 0C. Potassium t-butoxide (85 mg, 0.76 mmol) was added, and the reaction was allowed to proceed for 24 hours at this temperature. After the reaction was completed, a saturated aqueous solution of ammonium chloride (10 ml) and water (10 ml) were added. The solution was extracted with ethyl acetate (20 mL*3). The organic phases were combined, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel column chromatography (petroleum ether/ethyl acetate (v/v) = 5:1) to obtain a white solid 5a (810 mg, yield 62.3%).

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.

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. 13788-84-6, name is 3-Methyl-4-phenyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows., category: pyrazoles-derivatives

Example 4(2R)-N-hvdroxy-2-methyl-4-(3-methyl-4-phenyl-1 H-pyrazol-1-yl)-2-Step A: ethyl (2R)-2-methyl-4-(3-methyl-4-phenyl-1 H-pyrazol-1 -yl)-2-(methylsulfonvDbutanoateTo a solution of the 3-methyl-4-phenylpyrazole (400 mg, 2.53 mmol, 1 eq) in THF (25 mL) was added cesium carbonate (2.52 g, 7.70 mmol, 3 eq) and (R)-ethyl 4-bromo-2-methyl-2-(methylsulfonyl)butanoate (950 mg, 3.31 mmol, 1 .3 eq). The resulting suspension was heated to 70 C and stirred overnight. The reaction was filtered through celite, and the filter pad was washed with ethyl acetate (2x 100 mL). Combined filtrates were concentrated and the crude material was purified on a Analogix SF15-24g column using an eluant of ethyl acetate in heptane (0-80%) to give ethyl (2R)-2-methyl-4-(3-methyl-4-phenyl-1 H-pyrazol-1 -yl)-2- (methylsulfonyl)butanoate (178 mg, 19.3%). LC-MS M+H+ 365.1

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 13788-84-6.

Synthetic Route of 10010-93-2, The chemical industry reduces the impact on the environment during synthesis 10010-93-2, name is 3-Methyl-5-(trifluoromethyl)-1H-pyrazole, I believe this compound will play a more active role in future production and life.

In a 500 mL round bottom flask, 5-methyl-3-(trifluoromethyl)-1H-pyrazole (150 g,100 mmol), 4-bromo-1-fluoro-2-nitrobenzene (22 g, 100 mmol) and K2C03 (35 g, 250 mmol) were brought up in DMF (200 mL) and the mixture was stirred at 60 C for 6 hrs. The mixture was poured into H20 (200 mL) and extracted with Et20 (100 mL x 3). The combined organic phase was concentrated in vacuo. The crude product was obtained innearly quantitative yield (37 g) and was used for the next reaction without further purification. MS (ESI) 351.1 [M+H]+.

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-Methyl-5-(trifluoromethyl)-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Related Products of 500011-84-7, The chemical industry reduces the impact on the environment during synthesis 500011-84-7, name is 3-Bromo-1-(dimethylsulfamoyl)pyrazole, I believe this compound will play a more active role in future production and life.

To trifluoroacetic acid (70 mL) was slowly added [3-BROMO N, N DIMETHYL-1H] [PYRAZOLE-L-SULFONAMIDE] (i. e. the bromopyrazole product of Step B) (57.04 g). The reaction mixture was stirred at room temperature for 30 minutes and then concentrated at reduced pressure. The residue was taken up in hexane, insoluble solids were filtered off, and the hexane was evaporated to afford the crude product as an oil. The crude product was further purified by chromatography on silica gel using ethyl acetate/dichloromethane (10: 90) as eluent to afford an oil. The oil was taken up in dichloromethane, neutralized with aqueous sodium bicarbonate solution, extracted with dichloromethane [(3X),] dried over magnesium sulfate and concentrated to afford the title product as a white solid (25.9 g), m. p. [61-64 C.] 1H NMR (CDC13) 8 6.37 (d, 1H), 7.59 (d, 1H), 12.4 (br s, 1H).

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-1-(dimethylsulfamoyl)pyrazole, other downstream synthetic routes, hurry up and to see.