Day: January 5, 2021

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. 215610-30-3, name is 5-Methoxy-1H-pyrazole, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H6N2O

To a solution of 3-methoxy-lH-pyrazole (520 mg, 5.3 mmol, 1 equiv) in dry THF was added NaH (60 % in mineral oil, 1.06 g, 26.5 mmol, 5 equiv) at 0C. The reaction was stirred for 1 min at room temperature under nitrogen atmosphere. Then a solution of 2- isothiocyanato-l,3-dimethoxybenzene (1.56 g, 8 mmol, 1.5 equiv) in THF (5 mL) was added. The resulting mixture was stirred at room temperature for 4 hours. The reaction was quenched with H2O (30 mL) and extracted with EtOAc (3 * 50 mL). The combined organic extracts were washed with brine (30 mL), dried over anhydrous Na2S04, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (eluted with DCM/MeOH = 100/1) to afford the title compound N-(2,6- dimethoxyphenyl)-3-methoxy-lH-pyrazole-l -carbothioamide as a white solid (l.lg, 48% yield). LC-MS: m/z 294.1 (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.

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. 176969-34-9, name is 3-(Difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., Product Details of 176969-34-9

The compound of formula (III) was added to a 5% aqueous solution of sodium hydroxide, reacted at 60 C for 3 hours, and then hydrochloric acid was added to neutralize the pH to a weak acidity,(IV) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carboxylic acid;The compound of formula (IV) (40 mmol) was refluxed with thionyl chloride (0.4 mol) for 4 hours and distilled under reduced pressure to give(V) 1-methyl-3-difluoromethyl-1H-pyrazole-4-carbonyl chloride;

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.

These common heterocyclic compound, 10250-64-3, name is 1-Methyl-3-phenyl-1H-pyrazole-5-carboxylic acid, 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. SDS of cas: 10250-64-3

General procedure: To a solution of 19 (1.2 eq) and HOBt(1.4 eq) in DMF (0.5 M) were added EDCI (1.3 eq) and a solution of 15a-j or 16a-j (1.0 eq) in DMF (0.25 M), Et3N (3.5 eq) at 0 C. The reaction mixture was stirred at room temperature for 24 hours, then diluted in AcOEt. The organic phase was washed with water twice, saturated aqueous NaHCO3 three times, and brine, then dried over Na2SO4,filtered, and concentrated. The residue was purified by flash column chromatography to give intermediates 17a-j and 18a-j.

The synthetic route of 1-Methyl-3-phenyl-1H-pyrazole-5-carboxylic acid has been constantly updated, and we look forward to future research findings.

Electric Literature of 2075-46-9,Some common heterocyclic compound, 2075-46-9, name is 4-Nitro-1H-pyrazole, molecular formula is C3H3N3O2, 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.

Compound Ia (15.0 g, 133 mmol) was added to a suspension of palladium on carbon 10% (7.0 g, 6.65 mmol) in ethanol (100 mL). The mixture was shaken for 3 hours under hydrogen pressure (40 psi) at room temperature. The catalyst was removed by filtration through a pad of Celite and the solvent was evaporated. Compound Ib was obtained as a burgundy oil (10.5 g, 126 mmol, 95%) which was used in the following step without purification; GC/MS: m/z = 83 (100%).

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

Some common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, molecular formula is C4H6N2, 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. Formula: C4H6N2

A mixture of phosphoryl chloride (467 gm, 3.045 moles) and DMF was stirred for 1 hour at 0-5 C. The reaction is exothermic so temperature should be below 5 C. To this slowly added 1-methyl-1H-pyrazole (50 gm, 0.6090 moles) and stirred for 30 min at 0-5 C. Then slowly raised the temperature from 20-30 C. to 60-70 C. and stirred for 10-15 hours. Progress of the reaction was monitored by HPLC. The reaction mixture was cooled to 0-5 C., to this added ethyl acetate (250 ml), DM water (1 L) and aqueous ammonia solution (350 ml, pH-6 to 7). The reaction mixture was stirred for 1 hour at 20-30 C. The inorganic salt obtained was filtered off, washed with ethyl acetate (250 ml). The filtrate was transferred in to a separating funnel. The reaction mixture was allowed to settle. The organic layer was separated and aqueous layer was extracted with ethyl acetate (250 ml). The entire organic layer was transferred to the reaction vessel, stirred for 10-15 min and separated the final aqueous layer and organic layer. The combined organic layer having 1-methyl-1H-pyrazole-4-carbaldehyde and ethyl acetate was used as such for Step 2 without any purification or isolation at this step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 930-36-9, its application will become more common.

Electric Literature of 1280210-79-8, These common heterocyclic compound, 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, 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.

INTERMEDIATE 12; 2-(( clopropylsxrffonylV2.4.5.6-tetrahvdropyrrolof3.4-c]pyrazole trifluoroacetic acid salt Step A: fe^Bu 2-(cyclopen sulfonYl>2.6-^carboxylateTo a suspension of sodium hydride (60% dispersion in oil, 1.55 g, 38.7mmol) in anhydrous acetonitrile (200 mL) was added to terf-butyl 2,6-dihyclropyrrolo[3,4-c]pyrazole- 5(4H)-carboxylate (5.3 g, 25.5 mmol) in one portion under nitrogen at room temperature. The reaction mixture was stirred at room temperature for 2 h. To the resulting white suspension was slowly added cyclopropanesulfonyl chloride (6.9 g, 49.1 mmol) and the mixture was stirred at room temperature for 18 h, quenched with water (120 mL) and the layers were separated. The aqueous layer was then extracted with dichloromethane (2 x 100 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude material was purified on silica chromatography (300 g Biotage column) and eluted with 15-80% ethyl acetate in hexanes to yield the title compound and ter/-butyl 1- (cyclopentyisulfonyl)-2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-carboxylate as a white solid. LC/MS: 314.2(M+1).

The synthetic route of 1280210-79-8 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, molecular formula is C4H5IN2, 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. Quality Control of 4-Iodo-1-methyl-1H-pyrazole

To a cooled (-70 C) solution of cis-7-fluoro-N-methoxy-N-methyl-5-phenyl- 6,7-dihydro-5H- pyrrolo[l ,2-b] [l ,2,4]triazole-2-carboxamide (137 mg, 0.47 mmol) and l -methyl-4-iodo-lh-pyrazole (393 mg, 1.89 mmol) in tetrahydrofuran (10 mL) was added dropwise tert-butyllithium (1.3 M in hexane, 1.45 mL, 1.89 mmol) under a nitrogen atmosphere. The mixture was stirred at -70 C for 1 h and then quenched by addition of saturated aqueous ammonium chloride (10 mL). The resulting mixture was extracted with ethyl acetate (2 x 10 mL). The combined organic layers were concentrated under reduce pressure and the residue was purified by RP-HPLC (acetonitrile 27- 57%/0.05% hydrochloride in water) to afford cis racemic (l -methylpyrazol-4-yl)-[rac-(5R,7R)-7- fluoro-5-phenyl-6,7-dihydro-5H-pyrrolo[l ,2-b][l ,2,4]triazol-2-yl]methanone (53.4 mg, 36%) as a white solid. H NMR (400 MHz, CD3OD) delta 8.61 (s, 1H), 8.24 (s, 1H), 7.46 – 7.34 (m, 3H), 7.32 – 7.25 (m, 2H), 6.22 – 6.19 (m, 0.5H), 6.08 – 6.05 (m, 0.5H), 5.72 – 5.65 (m, 1H), 3.93 (s, 3H), 3.85 – 3.70 (m, 1H), 2.90 – 2.75 (m, 1H). LCMS RT= 0.791 min, m/z = 31 1.9 [M + H]+. LCMS (5 to 95% acetonitrile in water + 0.03%o trifluoacetic acid over 1.5 mins) retention time 0.791 min, ESI+ found [M+H] = 311.9.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 39806-90-1, 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. 57097-81-1, name is 3-Bromo-5-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Quality Control of 3-Bromo-5-methyl-1H-pyrazole

Step A: 5-(3-Bromo-5-methyl-lH-pyrazole-l -yl)-3-chloropyridazine To a solution of 3-bromo-5-methylpyrazole (0.4 g, 2.48 mmol) in DMF (5 mL) at room temperature was added KOtBu (0.279 g, 2.48 mmol) in one portion. To this mixture was added a solution of 3, 5-dichloropyridaine (0.37 g, 2.48 mmol) in DMF (5 mL). The reaction mixture was heated at 100 C for 1 h. The reaction mixture was cooled to room temperature, diluted with EtOAc (50 mL), washed with satd aq. NaHC03 (10 mL) and water (100 mL), the aqueous layers were separated and extracted with EtOAc (3 x 50 mL). The combined organic layers were washed with water (100 mL), brine (100 mL), dried over Na2S04, filtered and concentrated. The crude solid was purified by PTLC (50% EtOAc in hexanes) to afford 5-(3-bromo-5- methyl-lH-pyrazole-l -yl)-3-chloropyridazine, as a white solid. LCMS calc. = 272.95; found – 272.88 (M+H)+.

The synthetic route of 57097-81-1 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 83725-05-7, name is N-(5-Methyl-1H-pyrazol-3-yl)acetamide, 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 83725-05-7, HPLC of Formula: C6H9N3O

4.1.2 N-(5-methyl-4-nitro-1H-pyrazol-3-yl)acetamide (3) Compound 2 (4.5g, 32?mmol) was dissolved in 50?mL concentrated H2SO4, and the solution was cooled to -5?C. Concentrated HNO3 (2.3?mL, 32?mmol) was added dropwise and the mixture was maintained at -5?C for 3?h. The reaction mixture was added to 150?mL ice water slowly, and then white solid appeared with stirring. The solid washed by water and dried to give pure 3 (4.65?g, 25?mmol, 72% yield). Mp: 240-241?C; 1H NMR (400?MHz, DMSO-d6) delta 10.24 (s, 1H), 2.45 (s, 3H), 2.13 (s, 3H).

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, N-(5-Methyl-1H-pyrazol-3-yl)acetamide, other downstream synthetic routes, hurry up and to see.

Adding a certain compound to certain chemical reactions, such as: 1260243-04-6, name is Ethyl 5-amino-1H-pyrazole-4-carboxylate, 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 1260243-04-6, Safety of Ethyl 5-amino-1H-pyrazole-4-carboxylate

General procedure: Method I. A mixture of Py (4.4 ml) and AcOH (3.0 ml) was stirred and treated by the addition of 5-aminoazole1a-h (0.01 mol) and (2E)-(3-morpholin-4-yl)-acrylonitrile (2) (1.38 g, 0.01 mol). The obtained mixture was refluxed at 150C for 5 h. After refluxing, the mixture was cooled. The precipitate that formed was filtered off, washed with a small amount of EtOH, and dried. Method II. A solution (or suspension) of the appropriate aminoazole 1a-h (0.01 mol) in solvent (15 ml) (EtOH in the case of compound 3a, dioxane in the case of compounds 3b-h) was stirred at 50C and treated by adding 3,3-diethoxypropionitrile (4) (1.5 ml, 0.01 mol), then 36% HCl solution (0.86 ml, 0.01 mol). The reaction mixture was refluxed for 2.5-3 h, the suspension (or solution) was cooled to room temperature, and the target product was isolated by the method indicated for each particular compound.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 5-amino-1H-pyrazole-4-carboxylate, and friends who are interested can also refer to it.