Category: 3994-50-1

Some common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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: 3994-50-1

Pd / C (10%, 500 mg) was added to the column1-methyl-4-nitro-1H-pyrazole (1.90 g, 14.9 mmol)And methanol (25 mL)Hydrogen at room temperature overnight.Diatomaceous earth filter, dichloromethane washing filter cake,The filtrate was concentrated under reduced pressure, (Eluent: ethyl acetate / methanol (v / v) = 18/1) to give 1.35 g of a black solid, yield:83.7%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3994-50-1, its application will become more common.

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.

Reference of 3994-50-1,Some common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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 a portion (0.7 g) of the material so obtained, platinum oxide (0.05 g), ethyl acetate (5 ml) and ethanol (15 ml) was stirred under 3 atmospheres pressure of hydrogen for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated. There was thus obtained the required starting material (0.6 g); 1H NMR: (DMSOd6) 3.64 (s, 3H), 6.86 (s, IH), 6.97 (s, IH).

The synthetic route of 3994-50-1 has been constantly updated, and we look forward to future research findings.

Application of 3994-50-1, 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. 3994-50-1 name is 1-Methyl-4-nitro-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.

Example 1 5-chloro-1-methyl-4-nitro-1H-pyrazole To a 500 mL round bottom flask containing 4-nitro-1-H-pyrazole (5 g, 44.2 mmol) was added sodium hydroxide (1M, 200 mL) and dimethyl sulfate (31 mL, 330 mmol). The mixture was stirred at room temperature for 72 h and the mixture was extracted with CH2Cl2 (2*150 mL). The organic layer was separated and the solvent was distilled off to yield 1-methyl-4-nitro-1H-pyrazole as a white solid (4.30 g, 76%). Following WO 2007/99326, to a 500 mL 3-neck-round bottom flask was added 1-methyl-4-nitro-1H-pyrazole (4.30 g, 33.8 mmol) and THF (12 mL). The mixture was cooled to -78 C. and lithium hexamethyldisilazide in THF (1M, 88.4 mL, 90 mmol) was added dropwise via an addition funnel over 20 min. The brown mixture was stirred for 30 min and warmed to -45 C over 30 min. The mixture was cooled back down to -78 C. and hexachloroethane (10.5 g, 44.2 mmol) dissolved in THF (20 mL) was added via an addition funnel over 15 min. The mixture was stirred for 2.5 h, warmed from -78 C to -40 C and the reaction was monitored by LCMS. Upon completion of the reaction, the reaction was quenched with a solution of saturated NH4Cl (150 mL), and ethyl acetate (100 mL) was added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (100 mL). The combined organic layer was washed with water (150 mL), dried over Na2SO4 and the organic solvent was distilled off. The crude product was purified via flash chromatography (CH2Cl2/7% MeOH) to yield 5-chloro-1-methyl-4-nitro-1H-pyrazole as a white solid (1.40 g, 20%). 1H NMR (400 MHz, CDCl3) delta 8.13 (s, 1H), 3.92 (s, 3H); ESIMS m/z=162.0 (M+1)

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

Synthetic Route of 3994-50-1, A common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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.

A mixture of a portion (0.7 g) of the material so obtained, platinum oxide (0.05 g), ethyl acetate (5 ml) and ethanol (15 ml) was stirred under 3 atmospheres pressure of hydrogen for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated. There was thus obtained the required starting material (0.6 g); 1H NMR: (DMSOd6) 3.64 (s, 3H), 6.86 (s, 1H), 6.97 (s, 1H).

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 3994-50-1, 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. 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

A par flask was charged with 1-methyl-4-nitro-1H-pyrazole 15 (5.3 g, 41.0 mmol) and methanol (70 mL) followed by addition of Pd-C (50% w/w, 2.70 g). The flask was evacuated under vacuum and then purged with hydrogen. The reaction was stirred under hydrogen atmosphere (30 psi). The reaction was monitored by TLC. It was then filtered through sintered funnel with a pad of celite, washed with methanol and concentrated under reduced pressure to afford precursor-05 as a brown colored gummy solid (4.0 g, 99% yield) that was used as such for the next step without any further purification. ?H NMR (400 MHz, CDC13): 6 7.12 (s, 1H), 6.97 (s, IH), 3.78 (s, 3H), 2.87 (br s, 2H).

The chemical industry reduces the impact on the environment during synthesis 1-Methyl-4-nitro-1H-pyrazole. I believe this compound will play a more active role in future production and life.

Electric Literature of 3994-50-1,Some common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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 l-methyl-4-nitro-lH-pyrazole (1.10 g, 8.66 mmol) and Pd-C (10%, 190 mg) in EtOAc (20 mL) (containing 8 drops of 6N HC1) was hydrogenated under balloon H2 for 18 h. After being filtered through celite, the filtrate was concentrated in vacuo. The residue was dissolved in IN HC1 (20 mL), then washed with hexane, concentrated in vacuo to give 1 -methyl- lH-pyrazol-4-amine dihydrochloride as a solid (0.918 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-4-nitro-1H-pyrazole, its application will become more common.

Electric Literature of 3994-50-1,Some common heterocyclic compound, 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, molecular formula is C4H5N3O2, 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 N2 flushed pressure vial was added 5.6:1 of (S)-N-[( 15)-i -(6- chloropyridin2-yl)but-3-en- 1 -yl]-2-methylpropane-2-sulfinamide: (S)-N-[(iR)- 1 -(6-chloropyridin-2-yl)but-3 -en-i -yl] -2-methylpropane-2-sulfinamide (2. 18 g, 7.60 mmol), 1 -methyl-4-nitro- iH-pyrazole (0.966 g, 7.60 mmol), prepared as described in Intermediate 32A, di(adamant-i-yl)(butyl)phosphine (0.954 g, 2.66 mmol), PvOH (0.300 ml, 2.58 mmol), K2C03 (3.62 g, 26.2 mmol), Pd(OAc)2 (0.341 g, 1.52 mmol) and DMF (15.2 mL). The vial was purged with Ar. The vial was sealed and heated at 120 C overnight. Thereaction mixture was cooled to rt, partitioned between water and EtOAc, and the layers were separated. The aqueous layer was extracted with EtOAc (3x) and the organic layers were combined and concentrated. The crude product was purified using normal phase chromatography followed a second purification by reverse phase chromatography to give (S)-2-methyl-N-[( 1 R)- 1 -[6-( 1 -methyl-4-nitro- 1 H-pyrazol-5-yl)pyridin-2-yl]but-3-en- 1- yl]propane-2-sulfinamide (Diastereomer A) (0.275 g, 13%), MS(ESI) m/z: 274.4 (M+H) and (S)-2-methyl-N- [(1 S)- 1- [6-( 1 -methyl-4-nitro- 1 H-pyrazol-5 -yl)pyridin-2-yl]but-3-en-i-yl]propane-2-sulfinamide (Diastereomer B) (1.2 g, 57%); MS(ESI) m/z:274.4 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-4-nitro-1H-pyrazole, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 3994-50-1, name is 1-Methyl-4-nitro-1H-pyrazole, 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 3994-50-1, Recommanded Product: 1-Methyl-4-nitro-1H-pyrazole

A mixture of a portion (0.7 g) of the material so obtained, platinum oxide (0.05 g), ethyl acetate (5 ml) and ethanol (15 ml) was stirred under 3 atmospheres pressure of hydrogen for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated. There was thus obtained the required starting material (0.6 g); 1H NMR: (DMSOd6) 3.64 (s, 3H), 6.86 (s, IH), 6.97 (s, IH).

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.

Related Products of 3994-50-1, 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 3994-50-1 as follows.

General procedure: To a 8 mL glass vial equipped with a magnetic stirbar were sequentially added K2CO3 (207 mg, 1.5 mmol), the nitroazole substrate (0.50 mmol), aryl halide (0.50 mmol oras indicated), toluene (0.50 M or 1.0 M), Pd(OAc)2 (5.60mg, 0.025 mmol) and [PCy3H]BF4 (18.4 mg, 0.050 mmol).The reaction mixture was purged with nitrogen through aTeflon-lined cap. Then the cap was replaced with a newTeflon-lined solid cap. The reaction vial was moved to a preheatedreaction block. After stirring for 18 h at the indicatedtemperature, the reaction mixture was cooled to 25 C and concentrated. The residue was purified by flash column chromatography to provide the desired arylated product.

According to the analysis of related databases, 3994-50-1, the application of this compound in the production field has become more and more popular.