Day: February 25, 2021

Application of 31037-02-2,Some common heterocyclic compound, 31037-02-2, name is Ethyl 5-amino-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C7H11N3O2, 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 69 Preparation of ethyl 4-Hydroxy-1-methyl-6-oxo-6,7-dihydro-1H-pyrazolo-[3,4-b]pyridine-5-carboxylate A solution of sodium metal (12.7 g, 0.55 mol) in ethanol is treated at room temperature with ethyl 5-amino-1-methyl-4-pyrazolecarboxylate (25 g, 0.148 mol), stirred for 0.5 h, treated dropwise with a solution of diethyl malonate (80 ML, 0.52 mol in ethanol over a 0.5 h period, heated at reflux temperature for 56 h, cooled to room temperature, diluted with water, washed with ethyl acetate, acidified to PH 2 with HCl and filtered.The filtercake is washed sequentially with water, ethanol, ethyl acetate and toluene and dried in vacuo at 40 C. for 16 h to afford the title product as a white solid, 28.7 g (82% yield), identified by HNMR analysis.

The synthetic route of 31037-02-2 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. 100784-27-8, name is Methyl 3-chloro-1-methyl-5-sulfamoyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Application In Synthesis of Methyl 3-chloro-1-methyl-5-sulfamoyl-1H-pyrazole-4-carboxylate

To a mixture of 3-chloro-4-methoxycarbonyl-1-methylpyrazole-5-sulfonamide (7.0 g), 5.3 g anhydrous potassium carbonate and 50 ml of dry acetone, 2.8 g of n-butyl isocyanate was added at room temperature. The mixture was refluxed for 3 hours. (0092) After refluxing, acetone was evaporated under reduced pressure and the residue was dissolved in ice-water. After separation of a trace of water insolubles, the filtrate was acidified with hydrochloric acid and the crystals formed were filtered, washed with water and dried to obtain 5.2 g N-(n-butylcarbamoyl)-3-chloro-4-methoxycarbonyl-1-methylpyrazole-5-sulfonamide.

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.

Related Products of 632365-54-9, 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 632365-54-9 as follows.

A suspension of methyl 5-amino-1H-pyrazole-3-carboxylate (1.00 g, 7.086 mmol) and 1-(3,4-dimethoxyphenyl)-4,4,4-trifluorobutane-1,3-dione (2.153 g, 7.794 mmol) in ACETIC ACID (10 ml, 174.682 mmol) was heated to reflux (at 100 C.) for 5 hours. The mixture was cooled at room temperature, water was added and the precipitate collected by filtration, washed with water and dried under vacuum to give J1 as a green solid, 2.33 g (86% yield).

According to the analysis of related databases, 632365-54-9, the application of this compound in the production field has become more and more popular.

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 6645-69-8 as follows. COA of Formula: C5H5N3O4

To a solution of 2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)aniline(8; 0.14 g,0.58 mmol,1 equiv.)and 2-(4-nitro-lH-pyrazol-1-yl)acetic acid(3b- ; 0.10 g,0.58 mmol,1.0 equiv.)in pyridine(5 ml)slowly added P0C13 (0.49 g,3.21 mmol,7.8 equiv.)at 0 C. The reaction was further maintained at the same temperature for 15 minutes. The reaction mixture was then quenched into ice and the product was then extracted with ethyl acetate. The combined organic layer was washed by IN HC1 solution followed by brine solution,dried over sodium sulfate,filtered and concentrated under reduced pressure to get crude product. The crude product thus obtained was purified by column chromatography on silica gel with a mixture of ethyl acetate and n-hexane as an eluent to obtain 0.038 g of the title compound 1A-1-16 as off white solid.NMR(CDCI3): 8.42(d,J = 7.6 Hz,1H),8.32(s,1H),8.31(bs, 1H),8.24(s,1H),6.99(d,J = 11.6 Hz,1H),5.00(s,2H),3.36(q,J = 9.6 Hz,2H),2.43(s,3H).

According to the analysis of related databases, 6645-69-8, the application of this compound in the production field has become more and more popular.

Application of 1904-31-0,Some common heterocyclic compound, 1904-31-0, name is 1-Methyl-1H-pyrazol-3-amine, molecular formula is C4H7N3, 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.

General procedure: To a solution of benzoic acid which was obtained by hydrolysis of methyl esters 8 or 12A-E (0.22 mmol, 1.0 equiv), aminothiazole or imidazo[1,2-a]pyrazin-8-amine or aminopyrazole (0.33 mmol, 1.5 equiv), HATU (0.33 mmol, 1.5 equiv) and HOAt (0.33 mmol, 1.5 equiv) in DMF (2 mL) was added dropwise di(isopropyl)ethylamine (DIPEA) (0.12 mL, 0.67 mmol, 3 equiv). The reaction was run under microwave at 60 ¡ãC (40 W) for 30 min, and then cooled to room temperature and poured into brine. The aqueous layer was extracted with EtOAc. The combined organic layers were washed with brine, dried over anhydrous NaSO4 and concentrated. The residue was purified by chromatography (SiO2, petroleum ether/EtOAc = 4:1-1:1) to yield corresponding amides as white or yellow powder.

The synthetic route of 1904-31-0 has been constantly updated, and we look forward to future research findings.

Related Products of 288-13-1, A common heterocyclic compound, 288-13-1, name is 1H-Pyrazole, molecular formula is C3H4N2, 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.

4-Iodopyrazole (14).; A flask equipped with a nitrogen inlet, addition funnel, thermowell, and mechanical stirrer was charged with pyrazole (13, 450 g, 6.62 mol) and tetrahydrofuran (5 L). The mixture was cooled to 10 C. and N-iodosuccinimide (NIS, 1490 g, 6.62 mol, 1.0 equiv) was added in portions as a solid. The reaction mixture (slight suspension) was stirred at room 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 aqueous saturated sodium thiosulfate solution (2¡Á3 L) (organic layer lightens to a pale yellow), water (2¡Á3 L), and brine (2 L). The organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure to afford 4-iodopyrazole (14, 1138 g, 1284.1 g theoretical, 88.6%) as white to pale yellow solids after being dried in a vacuum oven at 30 C. overnight. For 14: 1H NMR (DMSO-d6, 400 MHz) delta ppm 13.17 (bs, 1H), 7.93 (bs,1H), 7.55 (bs,1H); C3H3IN2 (MW, 193.97), LCMS (EI) m/e 195 (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.

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. 40261-59-4, name is 1-Phenyl-1H-pyrazole-3-carbaldehyde, A new synthetic method of this compound is introduced below., Recommanded Product: 40261-59-4

Step 1 : l-(l-Phenyl-lH-pyrazol-3-yl)-propan-l-ol[0142] 1 -Phenyl- lH-pyrazole-3-carbaldehyde (779 mg, 4.53 mmol) was dissolved in anhydrous TEtaF (9 mL) and chilled in an ice bath. EtMgBr (3.0 M in Et20, 4.5 mL) was added dropwise. After 1.5 hours, the reaction mixture was allowed to warm to ambient temperature. TLC (2:1 hexanes:EtOAc indicated complete consumption of aldehyde starting material. The reaction mixture was quenched with water and extracted with EtOAc (2x). The EtOAc layers were washed with brine (Ix), dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography (2:1 hexanes: EtOAc) to provide the title compound (631 mg, 69%) as a yellow oil. 1H NMR (400 MHz, CDCl3) delta 7.85 (d, IH, J= 2.4 Hz), 7.65 (d, 2H, J= 7.6 Hz), 7.42 (t, 2H, J= 7.6 Hz), 7.27 (d, IH, J= 7.2 Hz), 6.38 (d, IH, J = 2.4 Hz), 4.79 (dd, IH, J= 12, 5.6 Hz), 2.38 (d, IH, J= 4.8 Hz), 1.98-1.81 (m, 2H), 1.01 (t, 3H, J= 7.2 Hz). MS (ES) m/z 203.1 (M+H+).

The synthetic route of 40261-59-4 has been constantly updated, and we look forward to future research findings.

Adding a certain compound to certain chemical reactions, such as: 930-36-9, name is 1-Methylpyrazole, 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 930-36-9, HPLC of Formula: C4H6N2

1) 1-Methyl-1H-pyrazole-4-carboaldehyde In an argon atmosphere, phosphorus oxychloride (65.3 mL) was added dropwise to N,N-dimethylformamide (54.2 mL) at 0C over 30 minutes, and the mixture was stirred at room temperature for 1 hour and 80C for 10 minutes. Subsequently, 1-methylpyrazole (25.0 g) was added dropwise to the reaction mixture over 30 minutes. The reaction mixture was stirred at 85C for 1 hour, at 100C for 3 hours, and at 115C for 1 hour, and then allowed to cool in air. The reaction mixture was added ice-water (1 L), and the mixture was stirred for 20 hours. The reaction mixture was partitioned between 1M aqueous sodium hydroxide (2 L) and chloroform, and the organic layer was dried over sodium sulfate anhydrate. After a filtration step, the solvent was evaporated under reduced pressure, and the residue was purified through silica gel column chromatography (chloroform – methanol), to thereby give 1-methyl-1H-pyrazole-4-carboaldehyde as an oily product (22.1 g, 66%). 1H-NMR(400MHz,CDCl3)delta:3.97(3H,s), 7.91(1H,s), 7.96(1H,s), 9.85(1H,s). ESI-MSm/z:111(M+H)+.

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Synthetic Route of 3920-50-1, 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 3920-50-1 as follows.

A mixture of 2-(4-{[2-amino-5-chloro-4-(trifluoromethyl)phenyl]amino}phenyl)ethanol (step 2 of Example 104, 2.28 g, 5.85 mmol) and 1H-pyrazole-3-carbaldehyde (562 mg, 2.85 mmol) in ethanol (35 ml) was stirred under reflux temperature for 1 h. The mixture was concentrated and dissolved in benzene (40 ml). To this solution was added lead tetraacetate (2.85 g, 6.44 mmol) at rt. After stirring at room temperature for 18 h, to the mixture were added saturated aqueous sodium hydrogencarbonate (50 ml) and ethyl acetate. The organic layer was separated and washed with brine, dried (Na2SO4) and concentrated. Purification by flash column chromatography eluting with dichloromethane/methanol (20:1 to 10:1), then dichloromethane/2-propanol (5:1) afforded 979 mg (41percent) of the title compound as a slight brown solid. [2276] 1H-NMR (CDCl3/CD3OD=4/1) delta: 8.12 (1H, br.s), 7.74 (1H, s), 7.59 (1H, br.s), 7.47 (2H, d, J=7.9 Hz), 7.34-7.30 (3H, m), 6.36 (1H, br.s), 3.87 (2H, br.t, J=6.8 Hz), 2.95 (2H, t, J=6.8 Hz). MS (ESI) m/z: 407 (MH+), 405 ([M-H]-).

According to the analysis of related databases, 3920-50-1, the application of this compound in the production field has become more and more popular.

Electric Literature of 89181-79-3, 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. 89181-79-3, name is 3-Amino-1-methyl-1H-pyrazole-4-carboxamide belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 3 -amino- 1 -methyl- lH-pyrazole-4-carboxamide from Example 20 Step C (100 mg, 0.71 mmol) in HOAc (0.6 mL) were added ethyl carbonocyanidate (77.8 mg, 0.79 mmol) and concentrated HC1 (0.06 mL). The mixture was stirred at 100 C for 5h. The mixture was concentrated and the residue was purified by silica gel chromatography eluting with 100/1 to 50/1 DCM:MeOH to afford ethyl 4-hydroxy-2-methyl-2H-pyrazolo[3,4-d]pyrimidine-6-carboxylate (58 mg, 36% yield) as a white solid. lH NMR (400 MHz, DMSO- 6) delta 12.06 (br s, 1H), 8.59 (s, 1H), 4.36 (q, J= 7.2 Hz, 2H), 4.06 (s, 3H), 1.35 (t, J= 7.2 Hz, 3H). LCMS (ESI) m/z 223 (M + H)+.

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-Amino-1-methyl-1H-pyrazole-4-carboxamide, other downstream synthetic routes, hurry up and to see.