Day: February 19, 2021

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. 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 4-Nitro-1H-pyrazole-3-carboxylic acid

Step 1 Thionyl chloride (9.2 mL) was added dropwise to a solution of 4-nitro-1H-pyrazole-3-carboxylic acid (19.77 g, 125.9 mmol) in methanol (200 mL) at 0C. The reaction mixture was stirred at room temperature overnight, and the solvent was evaporated under reduced pressure. Water was added to the residue, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated brine, dried and concentrated. The obtained crude crystals were washed with diisopropyl ether to give methyl 4-nitro-1H-pyrazole-5-carboxylate (17.8 g, 82%). 1H-NMR (300MHz, CDCl3) delta: 4.06 (3H, s), 8.50 (1H, s).

The synthetic route of 5334-40-7 has been constantly updated, and we look forward to future research findings.

Reference of 345637-71-0, A common heterocyclic compound, 345637-71-0, name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, molecular formula is C7H7F3N2O2, 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.

Step A: Preparation of 5-methyl-3-(trifluoromethyl)-lH-pyrazole-l -acetyl chloride A mixture of 5-methyl-3-(trifluoromethyl)-lH-pyrazole-l -acetic acid (5.2 g, 25 mmol) in dichloromethane (70 mL) and N,N-dimethylformamide (2 drops) was cooled to 0 C and oxalyl chloride (4.76 g, 37.5 mmol) in dichloromethane (10 mL) was added dropwise. The reaction mixture was stirred at room temperature for 16 h, and then concentrated under reduced pressure to give the title compound as a slightly yellowish solid (5.64 g). H NMR (CDC13): delta 6.38 (s, 1H), 5.27 (s, 2H), 2.31 (s, 3H).

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

Synthetic Route of 82560-12-1,Some common heterocyclic compound, 82560-12-1, name is 3-Amino-5-tert-butylpyrazole, molecular formula is C7H13N3, 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-tert-butyl-1H-pyrazol-5-amine (J-III) (1 equiv., 40 g) was dissolved in dilute HCl (120 mL HCl in 120 mL water) and NaNO2(1.03 equiv., 25 g in 100 mL) was added dropwise over 30 min. After stirring for 30 min the reaction mixture was neutralised with Na2CO3. A diazonium salt obtained by reacting KCN (2.4 equiv., 48 g), water (120 mL) and CuCN (1.12 equiv., 31 g) was added dropwise within 30 min to the reaction mixture, which was then stirred for a further 30 min at 75 C. After complete conversion the reaction mixture was extracted with EE (3¡Á500 mL), the combined phases were dried over sodium sulphate and the solvent was removed in vacuo. The column chromatography purification (SiO2, 20% EE/Hexane) of the residue yielded a white solid (J-IV) (6.5 g, 15.1% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Amino-5-tert-butylpyrazole, its application will become more common.

10199-57-2, name is 5-Methyl-1-phenyl-1H-pyrazole-3-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. Recommanded Product: 5-Methyl-1-phenyl-1H-pyrazole-3-carboxylic acid

General procedure: EDCI (1.1 equiv.) and HOBt (1.1 equiv) were added to a solution of the intermediate acid compound 1a-j (1 equiv.) in anhydrous DMF. The reaction mixture was stirred for 1h at ambient temperature, and the L-serine ester (1.1 equiv.) and DIEA (3 equiv.) were added. The solution was heated to 70C for 6h and then cooled to room temperature. The reaction mixture was poured into ice water, and the resulting solid was filtered and dried to give the desired compound.

The synthetic route of 10199-57-2 has been constantly updated, and we look forward to future research findings.

26308-42-9, name is 3-Ethyl-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. Computed Properties of C7H10N2O2

General procedure: Pyrazole acid 9a-k (3 mmol) and thionyl chloride (7.5 mmol)were successively added to 20 mL 1,2-dichloroethane, the mixturewere stirred under reflux for 3 h and then concentrated underreduced pressure, the crude products were added in drops into asolution of 5?a-f (5a-h) (3 mmol) and trimethylamine (6 mmol) inTHF (15 mL).The reaction mixturewas stirred under the 0 C for thenight. After reaction the mixture was poured in Na2CO3 solutionand aqueous phase was extracted with ethyl acetate (2 20 mL).The combined organic phase was washed with saturated salt water(2 20 mL), dried over anhydrous Na2SO4, and concentrated underreduced pressure and the residue was purified by silica gel columnchromatography.

The synthetic route of 26308-42-9 has been constantly updated, and we look forward to future research findings.

Related Products of 120068-79-3, A common heterocyclic compound, 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, molecular formula is C11H5Cl2F3N4, 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 1; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile with triethylamine hydrochloride, sodium trifluoromethylsulfinate and thionylchloride, in 6.5 molar equivalents of tolueneWithin a 3-neck, 50 ml. round bottom flask equipped with a magnetic stirrer bar and a thermometer were placed vacuum dried sodium trifluoromethylsulfinate (4.29 g, 27.5 mmol), vacuum dried triethylamine hydrochloride (5.16 g, 37.5 mmol), and 13 ml. an- hydrous toluene (6.5 molar equivalents relative to 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H-pyrazole-3-carbonitrile) under an argon atmosphere. After cooling to 00C to 5 0C with an ice bath, thionylchloride (3.57 g, 30 mmol) was added slowly while keeping the reaction temperature below 5 0C. After stirring for another 30 min, vacuum dried 5-amino-1-(2,6-dichloro-4-trifluoromethyl-phenyl)-1 H-pyrazole-3- carbonitrile (8.03 g, 25 mmol, 99 % purity) was added at 5 0C, and the reaction mixture was heated to 50 0C within 5 min by a preheated water bath. The temperature of 50 0C was kept for another 6 hours before quenching the reaction with 50 ml. of saturated NaHCO3 solution. The resulting suspension was diluted with 30 ml. of ethylacetate. After phase separa- tion the organic layer was washed once with saturated NaHCtheta3 solution and concentrated under reduced pressure until dryness. The crude product was crystallized from refluxing toluene (100 g) affording the title compound as a white crystalline powder (8.06 g, 70 % yield, 94 % purity by quantitative HPLC). 1H-NMR (Bruker DRX-500, d6- DMSO): delta [ppm]: 8.33 (s), 7.57 (s).; Example 17; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H-pyrazole-3- carbonitrile with triethylamine tosylate, sodium trifluoromethylsulfinate and thionylchlo- ride, in 6.5 molar equivalents of tolueneThe preparation procedure was conducted as described above for example 1. The crude product was crystallized from refluxing toluene (100 g) affording the title compound as a white crystalline powder (44 % yield, 76 % purity by quantitative HPLC). No formation of insoluble material (as with diethylamine tosylate as the amine acid complex, compare example C4 of Table 3) was observed.

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.

Electric Literature of 5334-40-7, 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. 5334-40-7 name is 4-Nitro-1H-pyrazole-3-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.

The 4-nitro-1H-pyrazole-3-carboxylic acid (20.0 g, 0.127 mmol) was dissolved in methanol (100 mL) and thionyl chloride (18.1 g, 0.152 mmol) was added , allowed to react for 2 hours at 25 C. , then heated to 60 C, and allowed to react for 2 hours. The reaction was concentrated in vacuo and methyl tert-butyl ether (80 mL) was added and filtered to give a white solid which was dried in vacuo to give the product (20.0 g, 92.1% yield).

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

Related Products of 1145-01-3, 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. 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 6 The preparation of 1-methyl-3,5-diphenylpyrazole Twenty parts of 3,5-diphenylpyrazole is dissolved in 100 parts xylene containing 7.26 parts of solid anhydrous sodium hydroxide. The reaction mixture is heated to 120C., and 13.8 parts of dimethyl sulfate are added. The reflux temperature drops to 95C., and after 15 minutes at 95C., a reaction mixture sample indicates no unreacted 3,5-diphenylpyrazole is remaining (tlc.) After 30 minutes, the reaction mixture is cooled to 80C. and 50 parts of water are added. Fifty percent aqueous sodium hydroxide is added to bring pH of aqueous phase to between 10 and 11. The organic layer is washed twice with 50 parts of water. For yield determination the xylene is removed in vacuo, producing 19.7 parts of an oil which crystallizes on seeding. Analysis of the product shows it to be 98.5% pure.

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, 3,5-Diphenyl-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 3920-50-1, 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. 3920-50-1, name is Pyrazole-3-carboxaldehyde belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a suspension of 0.60 g (6.24 mmol, 1.0 eq.) of 1H-pyrazole-3-carbaldehyde in 12 mL ofmethylene chloride at -40 ¡ãC under a nitrogen atmosphere was added 1.63 mL (9.37 mmol,1.5 eq.) of 1VN-diisopropylethyl amine, followed by 1.66 mL (9.37 mmol, 1.5 eq.) of[2- (chloromethoxy)ethyl]trimethylsilane. The mixture was allowed to warm to room temperature and stirred for 16 h. The reaction mixture was then diluted with 20 mL brine, and extracted with 3 x 30 mL of methylene chloride. The combined organic extracts were dried(Na2SO4), filtered, and the solvent was removed in vacuo. The residue was absorbed on CELITE? and purified by flash chromatography (Si02, eluting with a gradient of 0-30percent ethyl acetate/hexanes) to provide 1 g (66percent) of a mixture of 1-((2-(trimethylsilyl)ethoxy)methyl)- 1H-pyrazole-5 -carbaldehyde and 1 -((2-(trimethyl silyl)ethoxy)methyl)- 1H-pyrazole-3 – carbaldehyde in an approximately 1:1 ratio.

The synthetic route of Pyrazole-3-carboxaldehyde has been constantly updated, and we look forward to future research findings.

Synthetic Route of 127107-23-7,Some common heterocyclic compound, 127107-23-7, name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, molecular formula is C4H8ClN3, 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.

[00664] Synthesis of compound 1-94. To a 20-mL sealed microwave tube containing compound 112.5 (120 mg, 0.27 mmol, 1.00 equiv), 1 -methyl- lH-pyrazol-4-amine hydrochloride (77.7 mg, 0.58 mmol, 2.10 equiv) in 5 mL of isopropanol was added 0.02 mL of hydrochloric acid (4 M in dioxane) at room temperature. The reaction mixture was heated on microwave for 2.5 h at 140 C and resulting solids were collected by filtration. Crude collected was purified via flash column chromatography to give 72.2 mg (53%) of compound 1-94 as a off- white solid. LCMS (ES, m/z): 498 [M+H]+. 1H NMR(400MHz, <-DMSO): delta 8.94 (s, IH), 7.80 (s, IH), 7.46 (s, IH), 5.75-5.60 (s, IH), 4.65 (s, 2H), 34.08-3.95 (m, IH), 3.80 (s, 3H), 3.59 (t, 4H), 2.85 (s, 2H), 2.52 (s, 4H), 2.30-2.22 (m, IH), 2.10 (d, 2H), 1.92 (d, 2H), 1.55-1.32 (m, 4H), 1.28 (s, 6H). These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-1H-pyrazol-4-amine hydrochloride, its application will become more common.