Day: March 18, 2021

Electric Literature of 84547-84-2, 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. 84547-84-2 name is 4-Bromo-1-methyl-1H-pyrazole-5-carboxylic acid, 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.

Compound 22 (20 g) was dissolved in 100 mL of concentrated sulfuric acid.33 mL of concentrated nitric acid was slowly added dropwise in an ice water bath.After reacting for 16 h at room temperature, TLC showed a large amount of substrate remaining.After heating to 50 ¡ã C for 16 h, the substrate substantially disappeared.After cooling, the reaction solution was slowly added dropwise to 1 L of ice water.Extract with ethyl acetate and wash the organic phase several times with water until pH = 7.After concentration, column chromatography gave yellowSolid 23 (15 g).

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

Application of 288-13-1, 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. 288-13-1, name is 1H-Pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

4-Iodopyrazole (20) [0159] A flask equipped with a nitrogen inlet, an addition funnel, a thermowell, and a mechanical stirrer was charged with pyrazole (1, 450 g, 6.62 mol) and tetrahydrofuran (THF, 5 L) at ambient temperature. The mixture was then cooled to 10 C. and N-iodosuccinimide (NIS, 1490 g, 6.62 mol, 1.0 equiv) was added to the mixture in portions as a solid at approximately 10 C. The resulting reaction mixture was then stirred at ambient temperature for 1 hour (longer reaction times may be necessary depending on ambient temperature). The mixture was then filtered and the THF was removed under reduced pressure. The residue was suspended in ethyl acetate (6 L) and insoluble materials were filtered. The dark filtrate was sequentially washed with saturated aqueous sodium thiosulfate solution (2¡Á3 L) (organic layer lightens to a pale yellow), water (2¡Á3 L), and brine (2 L). The resulting organic layer was then dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford 4-iodopyrazole (1138 g, 1284.1 g theoretical, 88.6%) as a white to pale yellow solid after being dried in a vacuum oven at approximately 30 C. overnight. 1H NMR (400 MHz, DMSO-d6) delta 13.17 (bs, 1H), 7.93 (bs, 1H), 7.55 (bs, 1H) ppm; C3H31N2 (MW, 193.97), LCMS (EI) m/e 195 (M++H).

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

Electric Literature of 13808-65-6, 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. 13808-65-6 name is 4-Bromo-3-phenyl-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.

[0164] In a microwave tube was placed ethyl 2-bromothiazole-4-carboxylate (1058 mg, 4.48 mmol), 3-bromo-4-phenyl-1H-pyrrole (995 mg, 4.48 mmol), and K2C03 (929 mg, 6.72 mmol). The tube was sealed and DMSO (4 ml) was added. The mixture was heated at 120C for 4 h. The mixture was poured into vigorously stirred H20 (100 mL), and the solid was filtered, triturated with H20, and dried. The solid was re-dissolved in EtOAc and filtered. Some undissolved material was the hydrolized acid. The filtrate was concentrated and triturated with ca. 3% EtOAc/hexane to give ethyl 2-(4-bromo-3-phenyl- 1H-pyrazol- 1- yl)thiazole-4-carboxylate (1329 mg, 3.51 mmol, 78% yield).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Bromo-3-phenyl-1H-pyrazole, and friends who are interested can also refer to it.

Application of 70951-85-8, 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. 70951-85-8, name is 4-Bromo-1-(tert-butyl)-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a -78 0C solution of 4-bromo-l -7-butyI-lH-pyrazole (15 g, 74.3 mmol) in anhydrous THF (100 mL) was added /7-BuLi (2.5 M in hexane, 53 mL, 132 mmol) under N2, and the resulting mixture was stirred at -78C for 30 min. Excess dry ice was added at -78 0C, and the mixture was warmed slowly to RT and stirred overnight. The reaction was concentrated in vacuo, water was added and the pH was adjusted to pH 3 by the addition of 2N aq HCI. The aqueous solution was extracted with EtOAc. The extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The residue was recrystallized (EtO Ac-pet, ether) to give 1 -/-butyl- lH-pyrazole-4-carboxylic acid (8.0 g, 67 % yield). 1H NMR (300 MHz, CDCl3): ^ 8.10 (s, 1 H), 8.03 (s, 1 H), 1.64 (s, 9 H); MS (ESI) m/z: 168.9 [M+Hf.

The synthetic route of 4-Bromo-1-(tert-butyl)-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Related Products of 143426-52-2,Some common heterocyclic compound, 143426-52-2, name is 1-(4-(Chloromethyl)phenyl)-1H-pyrazole, molecular formula is C10H9ClN2, 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 mixture of 3- ( ( 3R, 4S ) -3-hydroxytetrahydro-2H-pyran-4-yl) -7-methyl-6- (4,4,5, 5-tetramethyl-l, 3, 2-dioxaborolan-2-yl ) – 2H-benzo [e] [1, 3] oxazin-4 (3H) -one (0.11 g) , l-(4- (chloromethyl) phenyl) -lH-pyrazole (0.06 g) , 2 M aqueous sodium carbonate solution (0.27 mL) and DME (3 mL) was addedtetrakis (triphenylphosphine) palladium (0) (0.02 g) at room temperature, and the mixture was stirred under an argonatmosphere at 90C overnight. The reaction mixture was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) and solidified with ethyl acetate to give the title compound (0.06 g) . NMR (300 MHz, DMSO-d6) delta 1.51-1.70 (1H, m) , 1.75-2.06 (1H, m) , 2.25 (3H, s) , 3.00 (1H, t, J = 10.4 Hz), 3.32-3.40 (1H, m) , 3.66 (1H, tt, J = 10.1, 5.0 Hz), 3.78-3.90 (2H, m) , 4.01 (2H, s), 4.04-4.23 (1H, m) , 5.09 (1H, d, J = 5.7 Hz), 5.18-5.42 (2H, m) , 6.52 (1H, dd, J = 2.5, 1.7 Hz), 6.90 (1H, s) , 7.21-7.27 (2H, m) , 7.57 (1H, s) , 7.70-7.72 (1H, m) , 7.73-7.78 (2H, m) , 8.43 (1H, d, J = 1.9 Hz).

The synthetic route of 143426-52-2 has been constantly updated, and we look forward to future research findings.

Application of 1254717-53-7, The chemical industry reduces the impact on the environment during synthesis 1254717-53-7, name is (5-(Trifluoromethyl)-1H-pyrazol-3-yl)methanamine, I believe this compound will play a more active role in future production and life.

(3-(Trifluoromethyl)-1 H-pyrazol-5-yl)methanamine (7 g, 42.4 mmol) was dissolved in DCM (7 mL) at room temperature, then to that TEA (5.86 mL, 72.4 mmol ) was added at room temperature and the mixture was stirred for 10 min and cooled to 0-5 ‘C. (Boc)20 (9.24 g, 42.4 mmol) was added drop wise to reaction mixture for 30 min and maintained for 3 h at 0-5 C. Progress of the reaction was monitored by the TLC (30 % ethyl acetate/n-hexane). On completion of the reaction, the reaction mixture was brought to room temperature for 2 h and the DCM was distilled off, the residue obtained was treated with water (50 mL) and extracted with ethyl acetate (100 mL). The combined organic layer was dried over sodium sulphate, and the solvent evaporated under vacuum. The obtained crude was purified with CC to yield tert-butyl (3-(trifluoromethyl)-1 H-pyrazol-5-yl)methylcarbamate as a white colored solid (5 g, 44 %).

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

Synthetic Route of 687635-04-7, 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 687635-04-7 as follows.

A solution of sodium hydrogen carbonate(0.364 g, 4.33 mmol) in H2O (3 ml) was slowly added to a stirredsolution of (3-(1H-pyrazol-1-yl)phenyl)methanamine sulfate (0.47 g, 1.73 mmol)in dichloromethane (8 ml) at 0C. A solution of cyanogen bromide (0.148 g, 4.52 mmol)in dichloromethane (3 ml) was then added to the reaction mixture at 0C. The mixturewas stirred at 0C for 30 minutes, allowed to come to ambient temperature andstirred for an additional 2 hours. The layers were separated, the dichloromethane extractwas washed with saturated sodium hydrogen carbonate solution (25 mL), saturatedsodium chloride solution (25 mL), dried over MgSO4 and evaporated in vacuoto a residue. The crude product was purified by flash silica chromatography,elution 20% ethyl acetate in heptane to give N-(3-(1H-pyrazol-1-yl)benzyl)cyanamide (0.261 g, 76%) as a whitesolid.1H NMR (400MHz, CDCl3) delta 7.93 (d, J = 2.5 Hz, 1H), 7.68 – 7.74 (m, 2H),7.62 (ddd, J = 8.1, 2.1, 0.8 Hz, 1H), 7.46 (t, J = 7.9 Hz, 1H),7.24 – 7.3 (m, 1H), 6.26 – 6.64 (m, 1H), 4.35 (s, 1H), 4.29 (d, J = 4.5Hz, 2H).

According to the analysis of related databases, 687635-04-7, the application of this compound in the production field has become more and more popular.

Related Products of 133228-21-4, 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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

19(1) 1-(Dimethylsulfamoyl)-4-fluoropyrazole 2.1 liters of fluorine gas (10% in N2) were bubbled, at 0-5 C., into a solution of 11.1 g of 1-(dimethylsulfamoyl)pyrazole [prepared as described in Example 1(1)] and 25.9 g of sodium acetate in 500 ml of a 9:1 by volume mixture of chloroform and acetic acid. The mixture was stirred for 2 hours, after which it was diluted with water. The organic layer was separated, washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by distillation under reduced pressure. The resulting residue was purified by column chromatography through silica gel, eluted with a 5:1 by volume mixture of hexane and ethyl acetate, to give 1.77 g (yield 14%) of the title compound as an oil.

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,N-Dimethyl-1H-pyrazole-1-sulfonamide, other downstream synthetic routes, hurry up and to see.

84547-84-2, name is 4-Bromo-1-methyl-1H-pyrazole-5-carboxylic acid, 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. HPLC of Formula: C5H5BrN2O2

To a solution of N-methyl-4-bromopyrazole-3-carboxylic acid (2.0 g), available from step A, in 65 mL of anhydrous DMF was added bromotripyrrolidinophosphonium hexafluorophosphate (PyBrop, 4.60 g), dimethyl amine (10 mL, 2.0 M in THF) and diisopropylethyl amine (5.2 mL) at 25 C. The mixture was stirred for 26 h, and concentrated under reduced pressure to an oily residue. This residue was treated with a 1.0 M NaOH aqueous solution, and extracted with ethyl acetate (50 mL x 4). The organic extracts were combined, washed with brine, and dried with anhydrous Na2SO4. Removal of solvents yielded an oil, which was purified by preparative thin layer chromatography, eluting with CH2CI2-MeOH (20: 1), to give 1.09 g of the amide product (48%, MH+ = 232.0).

The synthetic route of 84547-84-2 has been constantly updated, and we look forward to future research findings.

Electric Literature of 99662-34-7, 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. 99662-34-7 name is 4-Pyrazol-1-yl-benzaldehyde, 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.

To a cooled solution of 4-(pyrazol-l-yl)benzaldehyde (3.0 g, 0.017 mole) in methanol (20 mL) under N2, was added sodium borohydride (0.79 g, 0.02 mole) in portion wise. The reaction mixture was warmed to RT and stirred for 2 h. The reaction mixture was concentrated under vacuum, dissolved in ice cold water (75 mL) and extracted with ethyl acetate (100 mL x 2). Organic layer was washed with brine solution (50 mL), dried over Na2S04 and concentrated under vacuum to obtain the crude compound which was further purified by flash chromatography using ethyl acetate: n-hexane (40:60) to get l-(4- hydroxymethylphenyl) – 1 H-pyrazole . (0225) Yield: 2.4 g; 1H – NMR (DMSO- 6, 400 MHz) d ppm: 4.52 – 4.53 (d, J = 5.6 Hz, 2H), 5.23 – 5.26 (t, J = 5.7 Hz, 1H), 6.52 (s, 1H), 7.41 – 7.43 (d, J = 8.3 Hz, 2H), 7.72 (s, 1H), 7.77 – 7.79 (d, J = 8.3 Hz, 2H), 8.09 (d, J = 2.3 Hz, 1H); Mass (m/z): 175.1 (M+H)+.

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