Tag: M.W=0-100

288-13-1, 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. 288-13-1 name is 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.

Pyrazole (16g, 235mmol) was added in portions to sulfuric acid, 98%, (10OmL) keeping the temperature below 4O0C. To this solution was added nitric acid, 70%, (16mL) maintaining the temperature below 550C. After addition the reaction was heated at 550C for 3hours, and then cooled to O0C, before carefully adding to ice / water (40OmL) with stirring. This mixture was neutralized by the careful addition of aqueous 50% sodium hydroxide solution using external cooling and efficient stirring. The resultant solution was extracted with ethyl acetate (3x 30OmL), and the combined extracts were washed with brine (2x250mL) dried (Na2SO4) and concentrated in vacuo to yield a white solid, which was used without further purification, 24.74g, 93%.

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

288-13-1, A common compound: 288-13-1, name is 1H-Pyrazole, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

General procedure: In 50 mL round bottom flask, aryl halide (1.0 mmol), pyrazole (1.2 mmol), ligand (0.04 mmol), Cu2O (0.10 mmol), cesium carbonate (2.0 mmol), and dry solvent (20 mL) were placed under nitrogen atmosphere. The reaction mixture was heated in oil bath up to specified temperature under constant stirring for 20 h and then allowed to cool to room temperature. The reaction mixture was filtered through a plug of Celite in a fritted filter funnel and washed with ethyl acetate. If DMSO is used as solvent, it is extracted by washing the filtrate with 25 mL water for three times. The organic phase was dried over anhydrous MgSO4 and was removed under reduced pressure to provide the crude product which was purified by column chromatography on silica gel, using hexane and ethyl acetate in 3:1 ratio, respectively, as an eluent.

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, 1H-Pyrazole, other downstream synthetic routes, hurry up and to see.

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 2820-37-3 as follows. 2820-37-3

To a solution of crude reactant (249.5 mg, 0.629 mmol, theoretical amount) in anhydrous THF (5 mL) was added 3.4-dimethyl-lH-pyrazole (120.7 mg, 1.256 mmol) followed by potassium carbonate (173.6 mg, 1.256 mmol). The solution was stirred at 25 C overnight then the solution was diluted with ethyl acetate (200 mL). The resulting solution was washed with brine (2x100mL), dried over magnesium sulfate and concentrated in vacuo. The crude product was purified by silica gel chromatography (petroleum ether/ ethyl acetate =1 :3) to afford product (56 mg, 0.136 mmol, Yield=22% (2 steps)) as white solid. 1HNMR (400 MHz, CDC13) 5(ppm): 7.08 (1H, s), 4.77 (1H, AB), 4.76 (1H, AB), 2.55 (1H, t), 2.18 (3H, s), 1.00-2.20 (24H, m).0.67 (3H, s). LCMS: rt = 2.41 mm, m/z = 413.2 [M+H]+

According to the analysis of related databases, 2820-37-3, the application of this compound in the production field has become more and more popular.

35277-02-2, A common heterocyclic compound, 35277-02-2, name is 4-Fluoro-1H-pyrazole, molecular formula is C3H3FN2, 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 dry, nitrogen-purged 100 mL round-bottom flask equipped with a dropping funnel under argon atmosphere, NaH of 60% dispersion in mineral oil (674 mg, 16.9 mmol) was added in 60 mL of anhydrous THF solvent in the flask at ice-water bath, and 4-fluoro-1H-pyrazole (691 mg, 8.03 mmol) was stirred in over 30 min at the ice-water bath. Into the flask, the solution of (R)-3-bromo-2- hydroxy-2-methyl-N-(4-nitro-3-(trifluoromethyl)phenyl)propanamide (2.98 g, 8.03 mmol) in 10 mL of anhydrous THF was added through dropping funnel under argon atmosphere at the ice-water bath and stirred overnight at room temperature. After adding 1 mL of H2O, the reaction mixture was condensed under reduced pressure, and then dispersed into 50 mL of EtOAc, washed with 50 mL (x 2) water, evaporated, dried over anhydrous MgSO4, and evaporated to dryness. The mixture was purified with flash column chromatography as an eluent EtOAc/hexane = 1/2 to produce designed compound (2.01 g, 67%) as yellowish solid.MS (ESI) m/z 375.08 [M- H]-; 377.22 [M + H] +; 399.04 [M + Na]+;19F NMR (CDCl3, decoupled) d -60.13, -176.47; assigned by NOE and COSY; 1H NMR (400 MHz, CDCl3) d 9.14 (bs, 1H, NH), 8.01 (s, 1H), 7.97-7.91 (m, 2H), 7.38 (d, J = 3.6 Hz, 1H), 7.35 (d, J = 4.4 Hz, 1H), 5.95 (s, 1H, OH), 4.56 (d, J = 14.0 Hz, 1H), 4.17 (d, J = 14.0 Hz, 1H), 1.48 (s, 3H).

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

1453-58-3, Adding a certain compound to certain chemical reactions, such as: 1453-58-3, name is 3-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 1453-58-3.

Step 1 1-(4-Methoxy-phenyl)-3-methyl-1H-pyrazole: The title compound was prepared from 4-methoxyphenylboronic acid (1.85 g, 12.1 mmol), 3-methyl-1H-pyrazoles (0.5 g, 6.1 mmol) using the general procedure A with a yield of 30% (0.4 g); MS (APCI) m/z: 189 (M+1, 100).

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

1453-58-3, 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. 1453-58-3, name is 3-Methylpyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Step 3: Synthesis of R-1-[4-chloro-2-(3-methyl-pyrazol-1-yl)-phenyl]-2,2,2-trifluoro-ethanol. R-1-(2-bromo-4-chloro-phenyl)-2,2,2-trifluoro-ethanol (15.65 g, 54.06 mmol), 3-methylpyrazole (5.33 g, 65 mmol), CuI (2.06 g, 10.8 mmol), K2CO3 (15.7 g, 113.5 mmol), (1R,2R)-N,N’-dimethyl-cyclohexane-1,2-diamine (1.54 g, 10.8 mmol) and toluene (80 ml) were combined in a 250 ml pressure tube and heated to 130¡ã C. (oil bath temperature) for 12 h. The reaction mixture was diluted with ethyl acetate and washed with H2O (4*100 ml), brine, and dried over sodium sulfate. Removal of solvent gave a crude product, which was purified by ISCO column chromatography using 5-10percent ethyl acetate in hexane as solvent to get R-1-[4-chloro-2-(3-methyl-pyrazol-1-yl)-phenyl]-2,2,2-trifluoro-ethanol (13.5 g; 86percent).

The synthetic route of 3-Methylpyrazole has been constantly updated, and we look forward to future research findings.

35344-95-7, 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. 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, This compound has unique chemical properties. The synthetic route is as follows.

Step I. 1-({2-tert-butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazol-5-yl}sulfonyl)-1H-pyrazole-4-carbaldehyde2-tert-Butyl-1-[(4,4-difluorocyclohexyl)methyl]-1H-benzimidazole-5-sulfonyl chloride (0.8 g, 1.9 mmol) was added to a solution of 1H-pyrazole-4-carbaldehyde (0.6 g, 6.2 mmol) and DMAP (1.5 g, 12 mmol) in DCE (70 mL) at 0¡ã C. The reaction mixture was allowed to warm to ambient temperature and stirred for 3 h. The solvent was concentrated and the product was purified by flash chromatography on silica gel using DCM/EtOAc (1:1) as eluent to provide the title compound as white solid. Yield: 0.34 g (36percent); MS (ESI) (M+H)+=465.0.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

1120-82-7, name is (1H-Pyrazol-1-yl)methanol, 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. 1120-82-7

To a solution of lH-pyrazol-1-ylmethanol (4.33 mg, 44.1 mmol) in anhydrous dichloromethane (130 mL) was added dropwise a solution of phosphorus tribromide (4.2 mL, 44.1 mmol) in anhydrous dichloromethane (20 mL) at 00C. The mixture was stirred for 2.5 hours at room temperature. The mixture was evaporated, and the crude l-(bromomethyl)-lH-pyrazole was used in the next step without purification.

Statistics shows that 1120-82-7 is playing an increasingly important role. we look forward to future research findings about (1H-Pyrazol-1-yl)methanol.

A common heterocyclic compound, 1120-82-7, name is (1H-Pyrazol-1-yl)methanol, molecular formula is C4H6N2O, 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. 1120-82-7.

General procedure: To a solution of N-(3-cyano-4,5,6,7-tetrahydrobenzo[b]thiophen-2-yl)-3-hydroxybenzamide (12) (0.250g, 0.838mmol) in anhydrous THF (5mL), the corresponding alcohol (0.838mmol) and PPh3 (0.330g, 1.25mmol) were added. The reaction mixture was cooled on ice bath and DIAD (0.25mL, 1.25mmol) was added. The reaction was stirred overnight at room temperature. The solvent was evaporated under reduced pressure and the crude product was purified by flash chromatography.

The synthetic route of (1H-Pyrazol-1-yl)methanol has been constantly updated, and we look forward to future research findings.

1192-21-8, 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 1192-21-8 as follows.

Sparge a solution of 2-(2-chloro-4-pyridyi)-5-2-cyclopropoxy)ethyl]-6,6- dimethyi-thieno[2,3-c]pyrrol-4-one (13.9 g, 121 mmol), i-methyi-5-aminopyrazole (ii g, 113 rnrnoi), and sodium tert-butoxide (6.5 g, 68 mrnol) in toluene (150 mL) with nitrogen for 15 minutes. Treat the resulting mixture with (R)- I -[(Sp)-2- (dicyciohexyiphosphino)ferrocenyiiethyldi-tert-hutylphosphine (200 mg, 0.36 mmol) andbis(tri-o-toiyiphosphine)paliadium(0) (250 mg, 0.35 mmoi), Heat the reaction mixture to reflux for one hour. Cool the reaction to room temperature and dilute with EtOAc (500 mL), Wash the organic solution with water (300 mL), Separate and concentrate the organic phase under reduced pressure, Dissolve the residue inDCM (150 mL) and treat the solution with SILIAMETS Thiol (40 g, I .28 mrnol/g, 40-63 micron) and stir the mixture for four hours, Filter to remove the solid and concentrate the filtrate under reduced pressure to give the title compound I LI g (86%). MS (ink): 424 (M+i).

According to the analysis of related databases, 1-Methyl-1H-pyrazol-5-amine, the application of this compound in the production field has become more and more popular.