Tag: M.W:200-300

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. 34091-51-5, name is 5-Iodo-1-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Product Details of 34091-51-5

Production Example 18 1′-(4-Fluorophenyl)-2-methyl-1’H,2H-3,4′-bipyrazole Under a nitrogen atmosphere, a mixture of 5-iodo-1-methyl-1H-pyrazole (600 mg), [1-(4-fluorophenyl)-1H-pyrazol-4-yl]boronic acid (650 mg), tetrakistriphenylphosphine palladium (166 mg), 2 M sodium carbonate aqueous solution (2.9 mL), ethanol (3.0 mL) and toluene (6.0 mL) was stirred at 100 C. for 4 hours. Thereafter, water was added to the reaction solution, and the obtained mixture was then extracted with ethyl acetate. The organic layer was concentrated under a reduced pressure, and the residue was then purified by column chromatography (silica gel cartridge, hexane:ethyl acetate=9:1 to ethyl acetate), so as to obtain the title compound (450 mg) in the form of a light yellow solid. 1H NMR (600 MHz, CHLOROFORM-d) delta ppm 3.97 (s, 3H) 6.34 (d, J=1.83 Hz, 1H) 7.14-7.22 (m, 2H) 7.46-7.53 (m, 1H) 7.66-7.72 (m, 2H) 7.83 (s, 1H) 7.98 (s, 1H); MS (ESI pos.) m/z: 243 [M+H]+

The synthetic route of 34091-51-5 has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 231285-86-2, name is Ethyl 1-methyl-5-(trifluoromethyl)-1H-pyrazole-4-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. Formula: C8H9F3N2O2

ethyl 5- (trifluoromethyl) -1-methyl -1H- pyrazole-4- carboxylate and 5.5 mol% and ethyl 3-(trifluoromethyl) -1-methyl -1H- pyrazole-4-carboxylate 94 .5 mol% containing crude crystals 5.08g (0.02mol), water 7.58 g, 25 mass% sodium hydroxide aqueous solution 5.56 g (0.01 mol) were added to the 100ml round-bottomed flask, while stirring it was heated in an oil bath and reacted under reflux for 3 hours. After cooling to room temperature, 15 mass% hydrochloric acid 10.0 g (0.04 mol) was dropped from the dropping funnel and then toluene 50.0g was added. After cooling for 1 hour in an ice-water bath, using a 5C filter paper, suction filtered through a Kiriyama funnel, the filtrate was washed with 2 volumes of cold water. The obtained filtrate was dried under reduced pressure at 80 C. for 4 hours and got 3.94 g of crystals. When 19F-NMR analyzed this crystal, it was 3-(trifluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid: 99.9 mol%, 5-(trifluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid: 0.1 mol%. The toluene layer obtained by separating the filtrate into two layers, after concentrated in an evaporator, dried under reduced pressure at 80 C for 4 hours, got 0.28 g of crystals. When this crystal analyzed by NMR equally, it was 3-(trifluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid: 18.8 mole %, 5-(trifluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid 81.2 mol%.

The synthetic route of Ethyl 1-methyl-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate 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. 345637-71-0, name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, A new synthetic method of this compound is introduced below., Product Details of 345637-71-0

Step F: Preparation of N-methyl-2-[1-[[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl3acetyl]-4-piperidinyl]-N-[(1R)-1-phenylpropyl]-4-oxazolecarboxamide. 1,1-Dimethylethyl 4-[4-[[methyl[(1R)-1-phenylpropyl]amino]carbonyl]-2-oxazolyl]-1-piperidinecarboxylate (i.e. the product of Example 7, Step E) (209 mg, 0.49 mmol) was dissolved in 3 mL of a mixture of dichloromethane and methanol (1:1), and 1.23 mL (4.9 mmol) of 1 N HCl in dioxane was added. The reaction mixture was stirred at room temperature for 3 h. The solvents were evaporated under reduced pressure, and the residue was dissolved in 5 mL methanol and concentrated under reduced pressure (this procedure was repeated 3 times) to give the amine hydrochloride. To a solution of 5-methyl-3-(trifluoromethyl)-(1H)-pyrazole-1-acetic acid (89.5 mg, 0.43 mmol) and triethylamine (87 mg, 0.86 mmol) in 2 mL of dry acetonitrile was added a suspension of 0-benzotriazol-1-yl-N,N,N’,N’-tetramethyluronium hexafluorophosphate (178.25 mg. 0.47 mmol) in 2 mL acetonitrile and then a mixture of 140 mg (0.43 mmol) of the amine hydrochloride in 2 mL acetonitrile. The resulting mixture was stirred at room temperature for 3 h and concentrated under reduced pressure. The residue was purified by silica gel chromatography using 25-75 % of ethyl acetate in hexanes to give 84 mg of the title product, a compound of the present invention as an oil.1H NMR (CDCl3) delta 0.90-1.04 (m, 3H), 1.71-1.89 (m, 2H), 1.90-2.19 (m, 4H), 2.28-2.35 (m, 3H), 2.72 (s, 2H), 3.00-3.2 (m, 3H), 3.30-3.36 (t, IH), 3.87-4.35 (m, 2H), 4.98 (s, 2H), 5.92- 6.12 (m, IH), 6.3 (s, IH), 7.25-7.4 (m, 5H), 8.08-8.15 (br s, IH).

The synthetic route of 345637-71-0 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 1395443-04-5, A common heterocyclic compound, 1395443-04-5, name is 3-Iodo-1,4-dimethyl-1H-pyrazole, molecular formula is C5H7IN2, 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.

xA 125 mL round bottomed flask with stir bar and fitted with a septum was backfilled with nitrogen three times, after which THF (7.0 mL) was added followed by 3-iodo-1,4-dimethyl-1H-pyrazole (Preparative Step 1D) (917 mg, 4.13 mmol). To this solution was added dropwise a 1.3 M solution of iPrMgCl.LiCl in THF (5.45 mL) and the mixture was stirred for 1 h at room temperature. N-Methoxy-N,1-dimethylcyclopent-3-ene-1-carboxamide (600 mg, 3.55 mmol) in THF (5 mL) was added dropwise. After stirring for 2 h, the reaction mixture was quenched with saturated aqueous NH4Cl (20 mL) and extracted with DCM (3*25 mL). The combined extracts were dried (Na2SO4) and filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (EtOAc in heptane, 0-100%) to afford 500 mg (69%) of the title compound as a colorless oil. 1H NMR (400 MHz, CDCl3) delta 7.14 (s, 1H), 5.70-5.64 (m, 2H), 3.90 (s, 3H), 3.20-3.12 (m, 2H), 2.44-2.36 (m, 2H), 2.30 (s, 3H), 1.52 (s, 3H).

The synthetic route of 1395443-04-5 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 277299-70-4, name is 2-(3,4-Dimethylphenyl)-5-methyl-1H-pyrazol-3(2H)-one, 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 277299-70-4, Product Details of 277299-70-4

1) Take 2-nitro-6-bromophenol 12%, potassium carbonate 5% and benzyl bromide 7% in turn, and pour into 120 ml of acetonitrile solution for reflux reaction.After the reflux reaction was heated to 90 C and the temperature was maintained at 90 C for 3 hours, the reflux was continued.The reflux apparatus was cooled to room temperature, the resulting solution was filtered and concentrated to a dry solid, and the solid was placed in a 100 ml glass dish, and 40 ml of a triethylamine liquid was added to continuously heat the glass dish.Until white crystals appear on the solid surface,The glass dish is cooled, the solid is washed and dried with water, and the above materials are reserved for use; 2) The material obtained in the step 1) is dissolved in 100 ml of ethyl acetate, washed successively with 50 ml of water and 50 ml of a saturated sodium chloride solution, and after washing, anhydrous sodium sulfate crystals are added for moisture absorption and drying. The solution is filtered and concentrated to dry crystals, and the above materials are reserved for use; 3) Take 5% potassium carbonate, 6% 3-carboxybenzeneboronic acid, 5% palladium dichloride,20 ml of dioxane and 40 ml of water were placed in a 100 ml glass dish to react with the material prepared in step 2).After heating to 50 C in the reaction state, keep the temperature at 50 C and a pressure of 1 MPa was added to the nitrogen to carry out a protective reaction for four hours.Then, the temperature is lowered, the liquid in the glass dish is filtered, and after distilling off the dioxane under reduced pressure, water and a 1 mol/L hydrochloric acid solution are added to adjust the pH.The solution was filtered to obtain a solid, and placed in a 100 ml glass dish, 80 ml of isopropanol and an aqueous solution prepared in a ratio of 3:1 were added to carry out recrystallization, and the above materials were reserved for use; 4) The material prepared in the step 3) is placed in a 350 ml solution of ethyl acetate, 2% of palladium on carbon is placed in the solution, and hydrogen is reacted for 10 hours.The solution was filtered and concentrated to dry crystals, placed in a 100 ml glass dish, 80 ml of methanol was added to recrystallize, and the above materials were reserved for use;5) Take 2-(3,4-dimethylphenyl)-1,2-dihydro-5-methyl-3H-pyrazol-3-one 8% in order and mix in a ratio of 1:1:2 70ml of sodium nitrate,Sodium bicarbonate and an aqueous solution are placed in a 100 ml glass dish to react with the material prepared in step 4).After the reaction is completed, 20 ml of ethanolamine is added and hydrogen is introduced to carry out the reaction to obtain Eltrombopag;

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, 2-(3,4-Dimethylphenyl)-5-methyl-1H-pyrazol-3(2H)-one, other downstream synthetic routes, hurry up and to see.

Electric Literature of 84547-86-4, A common heterocyclic compound, 84547-86-4, name is 4-Bromo-1-methyl-1H-pyrazole-3-carboxylic acid, molecular formula is C5H5BrN2O2, 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.

[00474] EXAMPLE 42A. Synthesis of Compound 265.[00 4-bromo-N-methoxy-N,l-dimethyl-lH-pyrazole-3-carboxamide. A mixture of 4-bromo-l -methyl- lH-pyrazole-3-carboxylic acid (2.04 g, 10 mmol), 2-(lH-benzotriazole-l-yl)-l,l,3,3-tetramethyluronium tetrafluoroborate (3.21 g, 10 mmol), Nu,Omicron-dimethylhydroxylamine (1.22 g, 20 mmol) in N,N-Diisopropylethylamine (5 mL) and N,N-Dimethylformamide (20 mL) was stirred for 12 h at room temperature. The mixture was concentrated in vacuum, and the residue was purified by flash chromatography eluting with petroleum ether/ethyl acetate = 5: 1 to give the titled product as a colorless oil (2.4 g, 97%). LC/MS m/z 247 [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 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 1280210-79-8 as follows. name: tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate

A mixture of (1R,2R)-N1,N2-dimethylcyclohexane-1,2-diamine (25 uL, 0.158 mmol), copper (I) iodide (4.0 mg, 0.021 mmol), potassium phosphate tribasic (69.7 mg, 0.328 mmol), tert-butyl 4,6-dihydro-2H-pyrrolo[3,4-c]pyrazole-5-carboxylate (42.7 mg, 0.204 mmol) and [(3R,3aR,6R,6aS)-3-(1-allyl-6-chloro-5-iodo-imidazo[4,5-b]pyridin-2-yl)oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-6-yl]oxy-tert-butyl-dimethyl-silane (84 mg, 0.145 mmol) in dioxane (1.0 ml) was degassed (3×) and placed under nitrogen before being heated to 100 C. After 6 hours, the reaction mixture was diluted with EtOAc (30 ml), washed with water (20 ml), brine (10 mL), dried over MgSO4, filtered, and evaporated under reduced pressure to give an oil. The oil was purified on preparative silica plates (1×1000 u developed with 1:1 EtOAc/hexanes). The resulting solid (86.4 mg, 0.131 mmol) was dissolved in TFA (1.0 mL) and DCM (1.0 mL) and was stirred at room temperature. After 1 hour, the reaction mixture was evaporated to give an oil, and which was lyophilized from ethanol and benzene to give the title compound as a solid. LC-MS: calculated for C26H35ClN6O4Si 558.22 observed m/e: 559.27 (M+H)+ (Rt 1.15/2 min).

According to the analysis of related databases, 1280210-79-8, the application of this compound in the production field has become more and more popular.

Related Products of 60061-68-9, A common heterocyclic compound, 60061-68-9, name is 4-Bromo-3-methyl-5-(trifluoromethyl)-1H-pyrazole, molecular formula is C5H4BrF3N2, 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.

EXAMPLE 37; [4-(5-Methyl-3-trifluoromethyl-1H-pyrazol-4-vfl-phenviyacetonitrile; 37A. 4-Bromo-5-methyl-1 -(tetrahvdro-pyran-2-yl)-3-trifluoromethyl-1 H-pyrazole; To a solution of 4-bromo-5-methyl-3-trif.uorornethy.-1 H-pyrazole (1.4g, 6.2mmol, LOequiv) in chloroform (31ml) was added p-toluene sulphonic acid monohydrate (118mg, 0.62mmol, O.iequiv). The solution was cooled to EPO O0C and 3,4-dihydro-2H-pyran (0.85ml, 9.3mmol, 1.5equiv) was added drop-wise over 5 minutes. The mixture was allowed to warm to room temperature for 1 hour and the solvents were removed under reduced pressure. The crude mixture was purified by column chromatography (Sitheta2), eluting with 0->25% EtOAc-petrol over a linear gradient to afford the title compound 1.4 g (59%), LCMS (PS-A) R1 3.72 min [M+H]+ 314.

The synthetic route of 60061-68-9 has been constantly updated, and we look forward to future research findings.

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.

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.