Day: March 12, 2021

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.

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.

Synthetic Route of 152120-54-2, 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. 152120-54-2 name is tert-Butyl (((tert-butoxycarbonyl)amino)(1H-pyrazol-1-yl)methylene)carbamate, 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.

General procedure: Cbz-Arg(N,N-diBoc)-Val-Sta-NH(CH2)2Ph (69). A mixture of Cbz-Orn(N-Boc)-Val-Sta-NH(CH2)2Ph (52) (65 mg, 0.090 mmol) and 4M HCl in dioxane was allowed to stir for 1 h at 20C. The reaction mixture was concentrated to dryness in vacuo to obtain the crude residue as a on oil. The oil was dissolved in DCM (1 mL) and Et3N (6 muL, 0.043 mmol) was added. The solution was stirred vigorously for 5min. N,N?-bis-Boc-1-guanylpyrazole (13 mg, 0.042 mmol) was added and the solution was allowed to stir for 18 h at 20C. The reaction mixture was concentrated to dryness in vacuo to obtain a crude residue. The crude residue was subjected to a silica chromatography gradient eluting from 100% DCM to 10% MeOH/DCM to obtain Cbz-Arg(N,N-diBoc)-Val-Sta-NH(CH2)2Ph (69) as a solid (46 mg, 53%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, tert-Butyl (((tert-butoxycarbonyl)amino)(1H-pyrazol-1-yl)methylene)carbamate, and friends who are interested can also refer to it.

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.

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. 1191616-45-1, name is 4-(4-Bromophenyl)-1-methyl-1H-pyrazole, A new synthetic method of this compound is introduced below., SDS of cas: 1191616-45-1

Compound 6c (1.5g, 5.0mmol), 4-(4-bromophenyl)-1-methyl-1H-pyrazole (1.2g, 5.0mmol), catalyst Pd(dba) 2 (144mg, 0.25mmol) , Tri-tert-butylphosphine (101mg, 0.5mmol), sodium tert-butoxide (576mg, 6.0mmol) were dissolved in toluene (50ml), heated to 100 and stirred for 12 hours, TLC detection reaction, direct concentration column chromatography separation 1.6 g of off-white solid was obtained with a yield of 69.3%.

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.

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.

Related Products of 141573-95-7, 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. 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Preparation Example V.13-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylic acidA mixture of ethyl 3-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylate (1.4 g, 52 mmol) and aqueous sodium hydroxide solution (10% strength, 3.1 g, 8 mmol) was stirred at 60 C. for 2 h. The reaction mixture was cooled to room temperature, and the pH was then adjusted to 1 using concentrated hydrochloric acid. The reaction mixture was cooled further to 0 C., resulting in the precipitation of a solid. The precipitated solid was filtered off, washed with cyclohexane and dried under reduced pressure. This gave 3-difluoromethyl-1-methyl-1H-pyrazol-4-ylcarboxylic acid as a solid (amount: 0.8 g; yield: 87%). 1H-NMR (DMSO-d6): delta=3.9 (s, 2H), 7.2 (t, 1H), 8.35 ppm (s, 1H).

The chemical industry reduces the impact on the environment during synthesis Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate. I believe this compound will play a more active role in future production and life.

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. 30169-25-6, name is 3,6-Bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazine, A new synthetic method of this compound is introduced below., Quality Control of 3,6-Bis(3,5-dimethyl-1H-pyrazol-1-yl)-1,2,4,5-tetrazine

The synthesis and basic properties of the investigated compounds were described earlier in a previously published articles [27,34], except from molecule Tz2Pyr2 which was prepared by a standard procedure [23], stirring 1eq. of TzPyr2 with 1 eq. of piperazine in acetonitrile at 60, cool down after one hour and filtering off the pure product. The NMR of Tz2Pyr2 is provided in the ESI section. In all measurements, a solution of an investigated compound was prepared in a 0.1 M tetrabutylammonium tetrafluoroborate (Bu4NBF4; Sigma Aldrich 98%)/dichloromethane (Sigma Aldrich 99.9%) supporting electrolyte. Electrochemical analysis was performed for the solutions using a concentration of 2 mM of corresponding s-tetrazine derivative in supporting electrolyte, while for the spectroelectrochemical investigations a1 mM concentration was used.

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.

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.

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.