Tag: M.W:100-200

Application of 35691-93-1, A common heterocyclic compound, 35691-93-1, name is Ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate, molecular formula is C8H12N2O2, 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.

3,5-Dimethyl-1H-pyrazole-4-carboxylic acid ethyl ester (0.10 g, 1 mmol) (prepared as described in Tett 2002, 58, 18, p 3639), 3-bromo-5-trifluoromethyl-pyridine (0.16 g, 1 mmol), copper iodide (0.02 g, 0.2 mmol) and cesium carbonate (1.0 g, 3 mmol) were suspended in DMA (0.5 ml) and heated to 160 C. for 16 h. The reaction was diluted with EtOAc, washed repeatedly with ammonium hydroxide, brine and dried (Na2SO4) and concentrated. The residue was purified by flash column chromatography (EtOAc:n-heptane 1:9-2:8 gradient affording the title compound (0.07 g, 35%) as a yellow oil. MS: 314.2 (MH+).

The synthetic route of 35691-93-1 has been constantly updated, and we look forward to future research findings.

97421-13-1, name is 1-(tert-Butyl)-1H-pyrazol-4-amine, 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. Safety of 1-(tert-Butyl)-1H-pyrazol-4-amine

General procedure: A solution of 4-aminopyrazole 1b-d (1.03 mol) in THF (1400 ml) was cooled to 0, then DMAP (5.03 g, 0.041 mol) was added to the stirred solution, followed by slow addition of di(tert-butyl) dicarbonate (229 g, 1.05 mol)over 30 min. The mixture was maintained at the indicated temperature for 1 h, allowed to warm to the room temperature, and stirred for further 4-6 h. The reaction mixture was then heated at 40 for 1 h, evaporated, extracted with MTBE (800 ml). The obtained oily product was diluted with 3:2 MTBE-hexane mixture (300 ml), stirred, the precipitate that formed was filtered off and air dried. tert-Butyl (1-tert-butyl-1-pyrazol-4-yl)carbamate (2b).Yield 230 g (93%), violet powder, mp 72-73C. IR spectrum,nu, cm-1: 3273 (N-H), 1710 (C=O). 1H NMR spectrum,delta, ppm (J, Hz): 1.50 (9H, s, (CH3)3); 1.56 (9H, s, (CH3)3);6.25 (1H, s, NH); 7.33 (1H, s, H-5); 7.80 (1H, s, H-3).13C NMR spectrum, delta, ppm: 27.9; 29.2; 58.0; 79.7; 116.6;120.4; 128.9; 152.8. Mass spectrum, m/z (Irel, %): 240[+]+ (100). Found, %: C 60.02; H 8.71; N 17.44.C12H21N3O2. Calculated, %: C 60.23; H 8.84; N 17.56.

The synthetic route of 97421-13-1 has been constantly updated, and we look forward to future research findings.

Reference of 660845-30-7, 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. 660845-30-7, name is 5-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

In a 500 mL round-bottom flask, 6.0 g (31 mmol) of 5-chloro-3-(difluoromethyl)-1 -methyl-1 H- pyrazole-4-carbaldehyde were taken up in 30 mL of toluene. A solution of 2.4 g (62 mmol) of sodium hydroxide in 6 mL of water was added to the reaction mixture, followed by 103 mL of a 30% strength solution of hydrogen peroxide in water. During the addition, the temperature was kept below 37 C. The reaction mixture was then stirred at 50 C for 7 h. After cooling, the organic phase was extracted with 100 mL of water. The aqueous phase was acidified to pH 2 using dilute hydrochloric acid. The white precipitate formed was filtered off, washed twice with 20 mL of water and dried. This gave 3.2 g of 5-chloro-3-(difluoromethyl)-1 -methyl-1 H-pyrazole-4-carboxylic acid as a white solid. H NMR (400 MHz, DMSO-c/6) delta ppm : 3.78 (s, 3H); 7.12 (t, 1 H, JHF = 53.60 Hz); 13.19 (s, 1 H); IR (KBr): 1688 cm”1 (C=0); 2200-3200 cm”1 broad;

The synthetic route of 5-Chloro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carbaldehyde has been constantly updated, and we look forward to future research findings.

Synthetic Route of 79080-39-0, 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. 79080-39-0, name is 1-Methyl-1H-pyrazole-3-carbonitrile, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: LiH (35 mg, 4.44 mmol) was added to a stirring glyme (20 mL) solution of arachno-4,6-C2B7H13 (500 mg, 4.44 mmol) under N2 at room temperature. The solution was monitored by NMR until ?95% complete. The solution was then filtered through a frit under N2 to remove excess LiH. A glyme solution of 2,3,4,5,6-pentafluorobenzonitrile (2.8 mL, 22.2 mmol in 20 mL glyme) was added via syringe. The reaction mixture was stirred at reflux for 12 h, then cooled and filtered through a frit under N2. The resulting Li+[6-C6F5-nido-5,6,9-C3B7H9-] was not isolated, but instead stored as a stock solution until use. The concentration of the solution and the yield (81%, 0.09M) were determined by integrating the resonances in the 11B NMR spectrum of a B10H14 sample of known concentration and comparing that value with the integrated value of the resonances of the stock solution.

The chemical industry reduces the impact on the environment during synthesis 1-Methyl-1H-pyrazole-3-carbonitrile. I believe this compound will play a more active role in future production and life.

Synthetic Route of 5932-27-4, 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. 5932-27-4 name is Ethyl 1H-pyrazole-3-carboxylate, 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.

Step 1:; To a solution of 1 H-pyrazole-3-carboxylic acid ethyl ester 9a (500 mg, 3.57 mmol) in DMF (6.5 mL) is added K2C03 (542 mg, 3.93 mmol, 1 .10 equiv), Nal (1 .07 g, 7.14 mmol, 2.00 equiv) and 1 -bromo-2-fluoroethane (928 mg, 7.14 mmol, 2.00 equiv). The reaction mixture is stirred at 100 C for 48 h in a closed vial. The reaction is quenched with HCI 1 N (pH ~5-6), water is added and the mixture is extracted with EtOAc (5x). The organics are washed with brine, dried with anhydrous MgS04, filtered and concentrated. The crude mixture containing the 2 regioisomers is purified by prep HPLC. The appropriate fractions are combined, frozen and lyophilized to give 9g.UPLC-MS: 186.8 (M+H)+ 1H NMR (400 MHz, DMSO-d6) delta (ppm): 7.90 (d, 1 H, J = 2.4 Hz), 6.76 (d, 1 H, J = 2.4 Hz), 4.79 (dt, 2H, J = 47.3, 4.7 Hz), 4.53 (dt, 2H, J = 27.8, 4.7 Hz), 4.26 (q, 2H, J = 7.1 Hz), 1 .28 (t, 3H, J = 7.1 Hz).

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

Electric Literature of 105434-90-0, These common heterocyclic compound, 105434-90-0, name is Ethyl 5-amino-1H-pyrazole-3-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.

A solution of 5-Amino~lH-pyrazole-3~carboxylic acid ethyl ester (0.0775 g, 0.500 mmol), benzaldehyde (0.064 g, 0.60 mmol) and sodium triacetoxyborohydride (0.212 g, 1.00 mmol) in dichloroethane (5 cm3) and stirred over night at 6O0C. The solution was diluted with further dichloroethane (10 cm3), was washed with NaHCO3, until there was no further gas evolution, then with brine. The organic phase was dried over anhydrous Na2SO4, filtered, and solvent removed under reduced pressure to give a brown oil. The crude product was taken into acetonitrile (3 cm3) and purified by preparatory HPLC to give 5-benzylamino-lH-pyrazole-3- carboxylic acid ethyl ester.5-Benzylamino-lH-pyrazole-3-carboxylic acid ethyl ester was taken up in IM lithium hydroxide: tetrahydrofuran : methanol (1 : 5 : 1) (10 cm3)and heated at reflux over night. Solvent EPO was removed under reduced pressure and the crude product was acidified to pH 1 with 0.1M HCl and extracted with ethyl acetate (10 cm3). The organic phase was dried over anhydrous Na2SO4, filtered, and solvent removed under reduced pressure to give a brown, glassy solid. 1H (DMSO- d6): 7.35-7.2 (m, 5H, CH2C6H5), 6.0 (s, IH), 4.5 (s, 2H, CH2C6H5). m/z (ES+): 218 [M+H]+

Statistics shows that Ethyl 5-amino-1H-pyrazole-3-carboxylate is playing an increasingly important role. we look forward to future research findings about 105434-90-0.

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 3524-32-1 as follows. name: 5-Amino-1,3-dimethylpyrazole

A mixture of 5-amino-1,3-dimethyl-pyrazol (1.87 g, 16.8 mmol), 2,4-dichlorobenzaldehyde (2.95 g, 16.8 mmol, Fluorochem), and 2-mercapto-2-methylpropanoic acid (2.5 g, 20.8 mmol) was heated, in a microwave for about 60 min, at about 100 C. Subsequently, the reaction mixture was sealed and heated, for about 24 h, at about 150 C. After cooling to rt, THF (300 ml) was added, followed by EDC.HCl (4.25 g, 22 mmol) and DMAP (4-dimethylamino-pyridine, 0.2 g, 1.64 mmol). Subsequently, the reaction mixture was stirred for about 24 h, at rt. NaOH (2 M aqueous, 10 mL) and ethyl acetate (200 mL) were added. The layers were separated and the aqueous layer was extracted with ethyl acetate (50 mL). The combined organic layers were washed with water (2×50 mL), dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by column chromatography (SiO2, diethyl ether, followed by ethyl acetate) to afford 4-(2,4-dichlorophenyl)-1,3,6,6-tetramethyl-4,8-dihydropyrazolo[3,4-e][1,4]thiazepin-7-one (3.11 g, 8.4 mmol, 50%) as white solid: 1H-NMR (CDCl3, Bruker 400 MHz) delta 1.51 (3H, s); 1.64 (3H, s); 1.67 (3H, s); 3.78 (3H, s); 5.77 (1H, s); 7.17 (1H, dd, J=8.4, 2.0 Hz); 7.28 (1H, d, J=8.4 Hz); 7.41 (1H, d, J=2.0 Hz); H, m); 8.43 (1H, bs).

According to the analysis of related databases, 3524-32-1, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 23170-45-8, name is Methyl 3-methyl-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 23170-45-8, Recommanded Product: 23170-45-8

Methyl 3-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate. To a solution of methyl 3-methyl-1H-pyrazole-4-carboxylate (280 mg, 2 mmol) in DMF (30 mL) was added (1-bromoethyl)benzene (0.37 g, 2 mmol) and potassium carbonate (0.55 g, 4 mmol). The mixture was stirred at 20 C and stirred for 12 h. The solvent was evaporated in vacuo and the residue was purified by HPLC (Column: Dsisol, 10mu, C18, 250 mm x 50 mm; Mobile: acetonitrile (0.1% formic acid)-water (0.1% formic acid), acetonitrile from 30 to 70 in 80 minutes; oven: 20 C; flow rate: 50 mL/minute, wavelength: 214 nm) to give methyl 3-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate (90 mg, 19%, desired) and methyl 5-methyl-1-(1-phenylethyl)-1H-pyrazole-4-carboxylate (80 mg, 16%). The product was used for the next step directly.

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, Methyl 3-methyl-1H-pyrazole-4-carboxylate, other downstream synthetic routes, hurry up and to see.

Application of 25016-11-9, The chemical industry reduces the impact on the environment during synthesis 25016-11-9, name is 1-Methyl-1H-pyrazole-4-carbaldehyde, I believe this compound will play a more active role in future production and life.

General procedure: To the solution of 45.0 g aldehyde 10 (0.363 mol) in 225 cm3 pyridine, 45.4 g malonic acid (0.436 mol) and 0.900 g piperidine (10.9 mmol) were added. The resulting mixture was heated at 70 C for 3 days. The solvent was removed in vacuo, and the residue was triturated with H2O. The precipitate was filtered to give the product 11

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-pyrazole-4-carbaldehyde, 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. 29097-00-5, name is Methyl 3-amino-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., COA of Formula: C5H7N3O2

General procedure: A mixture of aminoazole 1c-e (1 mmol), acetoacetamide 2a,b,d (1 mmol), and aromatic aldehyde 3b,d-g (1 mmol) in 0.1 mL of DMF was heated to reflux for 10 min. After cooling acetone (10 mL) was added. The precipitate formed was filtered out to give the solid dihydropyrimidines 7a-e, which were washed with acetone and air dried.

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.