Tag: M.W=0-100

Adding a certain compound to certain chemical reactions, such as: 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, 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 1192-21-8, 1192-21-8

Example 194; N-(1-Methyl-1H-pyrazol-5-yl)-4-(3-phenyl-1,2,4-thiadiazol-5-yl)piperazine-1-carboxamide; (1) 2,2,2-Trichloroethyl (1-methyl-1H-pyrazol-5-yl)carbamate; To a solution of 1-methyl-1H-pyrazole-5-amine (1.00 g, 10.3 mmol) and pyridine (1.01 ml, 12.4 mmol) in tetrahydrofuran (34 ml) was added 2,2,2-trichloroethyl chloroformate (1.71 ml, 12.4 mmol) with ice-cooling and the mixture was stirred at room temperature for 1 hour. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane : ethyl acetate = 1 : 1) to obtain the desired product (1.43 g, 50.8percent) as an oil. 1H-NMR (CDCl3) delta; 3.78 (3H, s), 4.83 (2H, s), 6.21 (1H, br s), 7.15 (1H, br s), 7.43 – 7.44 (1H, m).

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, 1-Methyl-1H-pyrazol-5-amine, other downstream synthetic routes, hurry up and to see.

1453-58-3,Some common heterocyclic compound, 1453-58-3, name is 3-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.

After 3-methyl-1-pyrazole (2.0 g, 24.3 mmol) was dissolved in acetonitrile (25 mL), tert-butyl dicarbonate (6.5 g, 29.8 mmol) and 4-dimethylaminopyridine (0.31 g, 2.49 mmol) were added thereto at 0¡ãC, and the mixture was slowly warmed to room temperature and then stirred for 2 hours. Ethyl acetate (50 mL) was added to the reaction material, and the result was washed with a 1N aqueous hydrochloric acid solution (50 mL), a saturated aqueous sodium hydrogen carbonate solution (50 mL) and salted water (50 mL), dried with anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residue was purified using silica gel column chromatography (ethyl acetate/normal-hexane=1/4) to give tert-butyl 3-methyl-1H-pyrazole-1-carboxylate (4.13 g, 93percent). 1H-NMR (300 MHz, CDCl3) delta 1.64 (s, 9H), 2.34 (s, 3H), 6.17 (s, 1H), 7.96 (s, 1H).

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

Adding a certain compound to certain chemical reactions, such as: 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, 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 35344-95-7, 35344-95-7

lH-pyrazole-4-carbaldehyde (1.73 g, 18.00 mmol, 1.20 eq.) and Cs2C03 (9.78 g, 30.02 mmol, 2.00 eq.) were added to a solution of tert-butyl N-[3-(methanesulfonyloxy)cyclobutyl] carbamate (4 g, 15.08 mmol, 1.00 eq.) in DMF (100 mL). The resulting solution was stirred for 16 hours at 80 C and then diluted with 300 mL of water. The resulting solution was extracted with ethyl acetate (3×300 mL) and the organic layers combined. The resulting mixture was washed with brine (3×500 mL), dried over anhydrous sodium sulfate and concentrated under vacuum. The crude product was purified by Flash with the following conditions: Column, C18 silica gel; mobile phase, X:H20 Y_ACN=70/30 increasing to X:H20 Y_ACN=20/80 within 30 min; Detector, UV 254 nm. The isomers were separated by Prep-SFC with the following conditions (Prep SFC80-2): Column, Chiralpak IB, 2*25cm, 5um; mobile phase, CO2 (80%), IPA (20%); Detector, UV 220nm. This resulted in 1.2 g (30%) of tert-butyl N-trans-3-(4- formyl-lH-pyrazol-l-yl)cyclobutyl] carbamate as a white solid.

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-4-carbaldehyde, other downstream synthetic routes, hurry up and to see.

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. 25222-43-9, name is (1H-Pyrazol-4-yl)methanol, This compound has unique chemical properties. The synthetic route is as follows., 25222-43-9

General procedure: To a mixture of 3,6-dichloropyridazine (3.73 g, 25 mmol), 4(5)-Hydroxymethylimidazole (1.96 g, 20 mmol), and Cs2CO3 (8.14 g, 25 mmol) was added acetonitrile (80 mL). The mixture was refluxed for 3 h and was poured into H2O (200 mL). 1N HCl(aq) was added slowly until the pH is ca. 7-8. Then the aqueous layer was extracted with EtOAc (150 mL) and then CH2Cl2 (100 mL x 5). The combined organic layer was dried (Na2SO4) and filtered. After removal of solvent, the product was triturated with 10percent CH2Cl2/Et2O (30 mL x 3) to give 1.74 g of product. The filtrate was concentrated and was purified by column using 60-70-80percent EtOAc/(CH2Cl2/hexane=1/1) as the eluent to give 629 mg of prouct. Total 2.36g of D (53percent) was obtained.

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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. 35277-02-2 name is 4-Fluoro-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. 35277-02-2

Sodium hydride (700 mg, 17.4 mmol, 60% dispersion in mineral oil was added to a solution of fluoropyrazole (1000 mg, 11.6 mmol) in DMF (7 mL) at room temperature. The mixture was stirred at room temperature for 40 min. The mixture was then canulated to a 1-bromo-2-chloroethane (2000 mg, 13.9 mmol, in 1 mL of DMF). The mixture was heated to 60 C. for 12 h. Water (50 mL) was added to the reaction mixture and THF (2*200 mL) was added to extract the aqueous solution. The combined organic layer was dried, filtered, and concentrated to get a waxy oil residue. LC/MS and 1H-NMR indicated it’s the mixture of two products, compound 4c and compound 4d (1000 mg, 57.4% yield).

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

35277-02-2, A common compound: 35277-02-2, name is 4-Fluoro-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.

Step 1: A stirred suspension of methyl (1S,8R)-12-bromo-15-oxatetracyclo-[6.6.1 .02?7.09?4jpentadeca-2,4,6,9, 11,1 3-hexaene-4-carboxylate (NT-3a1; 480,00 mg: 1.45mmol: 1.00 eq.), methylboronic acid (173.53 mg; 2.90 mmol; 2.00 eq.), cesium carbonate (1 180.65 mg; 3.62 mmol; 2.50 eq.) and 1,1 -bis(diphenylphosphino)ferrocenej dichloro palladium(II) (106.06 mg; 0.14 mmol; 0.10 eq.) in 1,4-dioxane (57.98 ml) and methanol (16.10 ml) was heated to 80 C. After 1 h the reacting mixture was cooled to RT, filtered withadditional MeOH and concentrated. The brown residue was purified by column chromatography (40 G ISCO Gold) eluting with 1 0/b EtOAc in heptane to provide the desired methyl (1 R,8S)- 12-methyl-i 5-oxatetracyclo[6.6. 1. 02?7.09?4jpentadeca-2.4,6,9, 11,13- hexaene-4-carboxylate contaminated by inseparable methyl (1 R.8 S) 15 -oxatetracyclo[6.6,1 ,02?7,09?4lpentadeca-2,4,6,9, 11,1 3-hexaene-4-carboxylate (320 mg), Step 2: To a stirred suspension of methyl (1R,8S)-12-methyl-15-oxatetracyclo- [6.6.1 .02?7.09?4jpentadeca-2,4,6,9, 11,1 3-hexaene-4-carboxylate and methyl (1 R,8S) 15- oxatetracyclo [6.6.1.027. 14j pentadeca-2,4,6,9, 11,1 3-hexaene-4-carboxylate (320.00 mg; 1.20 mmol; 1.00 eq.), and N-bromosuccinimide (224.58 mg; 1.26 mmol; 1.05 eq.) in carbon tetrachloride (12.02 ml) was added AIBN (9.87 mg; 0.06 mmol; 0.05 eq.). The resultingmixture was heated to 75 C. After 3 h the reacting mixture was cooled to RT diluted with DCM, washed with sat. NaHCO3, dried over MgSO4, filtered and concentrated. The crude material was purified by column chromatography (12 G ISCO Gold) eluting with 10% EtOAc in heptane to provide methyl (1S,8R)-12-(bromomethyl)-15-oxatetracyclo- [6.6.1.027. ue 14j pentadeca-2,4,6,9, 11,1 3-hexaene-4-carboxylate contaminated by inseparablemethyl (1 S,SR)-i 2-(dibromomethyl)- 1 5-oxatetracyclo[6. 6.1 .02?7.09?4jpentadeca-2,4,6,9,11,1 3-hexaene-4-carboxylate (273 mg).

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, 4-Fluoro-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Adding some certain compound to certain chemical reactions, such as: 69843-13-6, name is 1-Methyl-1H-pyrazol-4-amine, 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 69843-13-6. 69843-13-6

To a solution of 1-methyl-1H-pyrazol-4-amine (500 mg, 5 mmol, 1.0 eq) in dioxane (10 mL) was added cyanamide (273 g, 6.5 mmol, 1.3 eq) and conc. HCl (1 mL). The reaction was stirred at 100 oC for 12 h. The solvent was removed under reduced pressure. The residue was recrystallized from the co-solvent of MeOH and Et2O. 1-(1-methyl-1H-pyrazol-4-yl)guanidine hydrochloride (600 mg, yield: 55%) was obtained as a yellow solid. ESI-MS (M+H)+: 140.1. 1H NMR (400 MHz, CD3OD) delta: 7.78 (s, 1H), 7.48 (s, 1H), 3.91 (s, 3H).

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 1-Methyl-1H-pyrazol-4-amine.

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. 25222-43-9, name is (1H-Pyrazol-4-yl)methanol, A new synthetic method of this compound is introduced below., 25222-43-9

6-(2,2-Diphenyl-ethylamino)-9-((lR,4S)-4-ethoxycarbonyloxy-cyclopent-2-enyl)-9H-purine-2- carboxylic acid methyl ester (4.91 g, 9.3 mmol), (lH-Pyrazol-4-yl)-methanol (1.0 g, 10.2 mmol) and PhyP (0.73 g, 2.8 mmol) are dissolved in dry, deoxygenated tetrahydrofuran under EPO argon. Pd2(dba)3 (0.85 g, 0.93 mmol) is added to the reaction mixture. The reaction mixture is heated at 45¡ã C for 1 hour. The solvent is removed in vacuo. The title material is obtained by flash column chromatography (silica, eluent 0percent MeOH to 3percent MeOH in DCM) (MH+ 536.42).

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.

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.

To a solution of 1H-pyrazole-4-carbaldehyde (70 mg, 728 mumol) in MeCN (5 mL) was added 1-(bromomethyl)-4-chlorobenzene (149 mg, 728 mumol) and cesium carbonate (472 mg, 1.45 mmol). The mixture was stirred at r.t. for 2h. The mixture was concentrated, diluted with EA and water. The organic phase was washed with brine (10 mL x 2), dried over Na2SO4and concentrated to give 1-(4-chlorobenzyl)-1H- pyrazole-4-carbaldehyde (162 mg, 101 percent) as a white solid, which was used in the next step without further purification

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28466-26-4, Name is 4-Aminopyrazole, 28466-26-4, 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.

46 mg (0.53 mmol) of 4-amino-1H-pyrazole were dissolved in 2.4 ml of DMF and stirred with 21 mg (0.5 mmol) of sodium hydride (60% in paraffin) at 23 C. for 30 minutes. 100 mg (0.18 mmol) of 5-[4-chloro-3-(trifluoromethyl)benzyl]-2-(methylsulphonyl)-6-(trifluoromethyl)pyrimidin-4(3H)-one (Example 39A, purity 77%) were then added, and the mixture was stirred at 120 C. for 30 minutes. The mixture was then purified directly by preparative HPLC [column: Chromatorex C18 10 mum, 250¡Á30 mm; flow rate: 50 ml/min; run time: 35 min; detection: 210 nm; injection after 3 min of run time; mobile phase A: acetonitrile, mobile phase B: water; gradient: 10% A (5.00 min)?80% A (25.00 min)?95% A (25.50-30.00 min)?10% A (30.50-35.00 min)]. The product-containing fractions were combined and concentrated. The residue was re-purified by preparative thin-layer chromatography (silica gel, mobile phase dichloromethane/methanol 20:1). This gave 41 mg (53% of theory) of the title compound.

Statistics shows that 4-Aminopyrazole is playing an increasingly important role. we look forward to future research findings about 28466-26-4.