Tag: M.W=300-400

A common compound: 162758-35-2, name is 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below. 162758-35-2

To a solution of the compound NDS-100226 (76 mg, 0.20 mmol)in dry dichloromethane, was added N-(3-Dimethylaminopropyl)-N’-ethylcarbodiimide hydrochloride (EDC.HC1, 40 mg, 0.26 mmol), Hydroxybenzotriazole (HOBt, 35 mg, 0.26 mmol) and diisopropylethyl amine (0.1 mL, 0.60 mmol) at 0C. Then the amine 3 was added and stirred at RT for 6 h. To the reaction mixture water was added and the organic layer was separated, washed with saturated NaHC03, IN HQ, dried over Na2S04 and concentrated under reduced pressure. This crude mixture was purified by column chromatography to give the title compound NDS-100240 (90 mg) as a white fluffy solid in 89% yield. NMR (400 MHz, CDQ3): delta 7.44 (d, J = 1.8 Hz, 1H), 7.32-7.29 (m, 4H), 7.06 (d, J = 8.3 Hz, 2H), 3.21 (t, J = 6.0 Hz, 411), 2.37 (s, 3H), 0.97 (t, J = 6.3 Hz, 4H), 0.10 (s, 6H) ); 13C NMR (100 MHz, CDC13): 6 159.9, 144.4, 142.9, 135.9 (2C), 134.9, 132.9, 130.8 (2C), 130.5, 130.3, 128.9 (2C), 127.8, 127.2, 1 18.2, 55.4, 13.2, 9.3, -3.5 (2C).

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, 162758-35-2, other downstream synthetic routes, hurry up and to see.

162758-35-2, name is 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-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. 162758-35-2

General procedure: To a mixture of carboxylic acid (1 mmol), EDC¡¤HCl (1.2 mmol) and HOBt (1.2 mmol) in dry dichloromethane (10 mL) was added a mixture of amine (1 mmol) and triethyl amine (1.5 mmol) in dichloromethane (5 mL) at 0 C. The mixture was stirred at room temperature till the completion of reaction (judged by TLC). The reaction mixture was diluted with additional DCM (20 mL). The organic layer was washed with water, brine and dried (Na2SO4). Concentration and purification over silica gel (100-200 mesh) afforded the desired compound.

Statistics shows that 162758-35-2 is playing an increasingly important role. we look forward to future research findings about 5-(4-Chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid.

Some 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, 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. 120068-79-3

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 12; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H-pyrazole-3- carbonitrile with trimethylamine tosylate, sodium trifluoromethylsulfinate and thionyl- chloride, 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 (76 % yield, 96 % purity by quantitative HPLC).; Example 14; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile with trimethylamine tosylate, sodium trifluoromethylsulfinate and thionylchloride, in 6.5 molar equivalents of tolueneThe preparation procedure was conducted as described above for example 11. The crude product was crystallized from refluxing toluene (100 g) affording the title com- pound as a white crystalline powder (73 % yield, 98 % purity by quantitative HPLC).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 120068-79-3, its application will become more common.

120068-79-3, A common compound: 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

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 2; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile with triethylamine hydrochloride, potassium trifluoromethylsulfinate and thionylchlorideWithin a 3-neck, 50 ml. round bottom flask equipped with a magnetic stirrer bar and a thermometer were placed vacuum dried potassium trifluoromethylsulfinate (4.73 g, 27.5 mmol), vacuum dried triethylamine hydrochloride (5.16 g, 37.5 mmol), thionylchloride (3.57 g, 30 mmol), and 15 ml. anhydrous toluene under an argon atmosphere. The reaction is further conducted as described above for example 1. EPO The crude product was crystallized from refluxing chlorobenzene (100 g) affording the title compound as a white crystalline powder (7.44 g, 66 % yield, 96 % purity by quantitative HPLC). 1H-NMR (Bruker DRX-500, d6-DMSO): delta [ppm]: 8.33 (s), 7.57 (s).; Example 10; Sulfinylation of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile with triethylamine hydrochloride, potassium trifluoromethylsulfinate and thionylchloride, in 4.5 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 potassium trifluoromethylsulfinate (5.16 g, 30 mmol), vacuum dried triethylamine hydrochloride (5.16 g, 37.5 mmol), and 10.4 g anhydrous toluene (4.5 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 external cooling, thionylchloride (3.57 g, 30 mmol) was EPO added within 15 min 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 kept at 5 0C for 60 min and then heated to 35 0C within 45 min. The temperature of 35 0C was kept for 3 hours before adding 4.6 g of toluene. After another 7 hours at 35 0C the reaction was quenched with 20 g of sodium hydroxide solution (10 wt.%).The resulting suspension was diluted with 30 ml. of ethylacetate. After phase separation the organic layer was washed once with sodium hydroxide solution (10 wt.%). After phase separation, the organic layer was analyzed by quantitative HPLC (80.4 % yield). The crude product was crystallized from a mixture of ethylacetate and toluene affording the title compound as a white crystalline powder (7.98 g, 73 % yield, 98 % purity by quantitative HPLC).; Example 11; Sulfinylation of 5-amino-1 -[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile with thionylchloride, triethylamine hydrochloride and dosage of potassium trifluoromethylsulfinateWithin a 750 mL reactor with a mechanical stirrer and a thermometer were placed vac- uum dried triethylamine hydrochloride (51.1 g, 368 mmol), 147 g anhydrous toluene(6.5 molar equivalents relative to 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-1 H- pyrazole-3-carbonitrile), and thionylchloride (35.7 g, 294 mmol) under an argon atmosphere. After cooling to 00C to 5 0C with external cooling, vacuum dried potassium trifluoromethylsulfinate (50.4 g, 296 mmol) was added in three equal portions every 10 min while keeping the reaction temperature be…

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-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, 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. 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, A new synthetic method of this compound is introduced below., 120068-79-3

General procedure: A mixture of compound A (5 mmol) and corresponding benzaldehyde (5 mmol) in 10 mL ethanol was refluxed for 24 hours in a reaction flask wrapped up by silver paper. Upon the reactions completed (monitored by TLC), tawny solids were obtained through suction filtration. The precipitates were washed with ethanol (5 mLx3) and recrystallized from ethanol with 50-84% yields.

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.

120068-79-3, 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 120068-79-3 as follows.

5-Amino-3-cyano-4-dichlorofluoromethylthio-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole, m.p. 178-180C in the form of a white solid, after purification by chromatography eluding with diethyl ether/hexane (1:1); from 5-amino-3-cyano-1-(2,6-dichloro-4-trifluoromethylphenyl)pyrazole. By proceeding in a similar manner but employing a molar equivalent of pyridine in the reaction solution there was obtained:

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 120068-79-3, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 17635-44-8, name is 3,4,5-Tribromopyrazole, 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 17635-44-8, 17635-44-8

EXAMPLE 1 Preparation of Ethyl 3,4,5-Tribromopyrazole-1-acetate A quantity (92 gm., 0.3 mole) 3,4,5-tribromopyrazole was added with vigorous stirring to a solution of 7.1 gm. sodium (0.31 mole) in 300 ml. absolute ethanol. After the mixing was complete, 100 gm. (0.6 mole) ethyl bromoacetate was added dropwise while stirring was continued. The mixture was diluted with 200 ml. absolute ethanol and this reaction mixture was stirred at about 25 C. for about 18 hrs. After removing most of the ethanol by evaporation under reduced pressure, 100 ml. of 6 N hydrochloric acid was added to the residue, and this aqueous acid mixture was made alkaline with solid sodium carbonate. The aqueous layer was separated and extracted with three 60-ml, portions of ether. The ether extracts were combined, washed with three 40-ml. portions of water, and dried with anhydrous magnesium sulfate. After removing the ether by evaporation under reduced pressure, there was obtained a white solid. Recrystallization from technical hexane (Skellysolve B, a mixture of isomeric hexanes having a boiling range between 61 C. and 69 C.) gave 96.0 gm. of ethyl 3,4,5-tribromopyrazole-1-acetate having a melting point at 101 to 103 C. Analysis: Calc’d. for C7 H7 Br3 N2 O2: C, 21.51; H, 1.81; N, 7.17; Br, 61.33. Found: C, 21.79; H, 1.62; N, 6.96; Br, 61.56.

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, 3,4,5-Tribromopyrazole, other downstream synthetic routes, hurry up and to see.

17635-44-8, 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 17635-44-8 as follows.

The bromopyrazole 1c was prepared according to the published procedure [19]. Single crystals of (1c)2?HBr were grown from the reaction mixture at r. t. In a second crop crystals containing 1c, HBr, and Br2 in the ratio of 1 : 1 : 0.5 were obtained from this solution at r. t.

According to the analysis of related databases, 3,4,5-Tribromopyrazole, the application of this compound in the production field has become more and more popular.

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. 120068-79-3, name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, A new synthetic method of this compound is introduced below., 120068-79-3

General procedure: A mixture of compound A (5 mmol) and corresponding benzaldehyde (5 mmol) in 10 mL ethanol was refluxed for 24 hours in a reaction flask wrapped up by silver paper. Upon the reactions completed (monitored by TLC), tawny solids were obtained through suction filtration. The precipitates were washed with ethanol (5 mLx3) and recrystallized from ethanol with 50-84% yields.

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.

120068-79-3, Name is 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile, 120068-79-3, 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.

In a reaction vessel equipped with a mechanical stirrer, a thermometer, a dropping device, and a reflux condenser, nitrogen in the reaction vessel was thoroughly replaced with nitrogen, and then 176 g (0.55 mol) 5-amino-3-cyano-1- (2,6-dichloro-4-trifluoromethylphenyl)pyrazole and 800g chloroform solution (the solution was fully dried over anhydrous sodium sulfate, the amount of desiccant is 500% of the theoretical amount required for the formation of complete hydrate from the free water of sodium sulfate and the system, and the desiccant is filtered and filtered) an additional 130 g (0.60 mol) of the dried salt of p-toluenesulfonic acid dimethylamine, the test solution has a water content of 250ppm (system contains about 0.28g, S Jie 15.4mmol7jO, add 1.18g (7.7mmol) of phosphorus oxychloride,Stirring at room temperature 0.5h, the test solution has a water content of less than 50ppm, achieve moisture control standards, the system was cooled to 0 C, 88.5g (0.58mol) of trifluoromethanesulfonyl chloride was added dropwise and evaporated to dryness, and the temperature was raised to the reflux temperature at the end of the dropwise addition. The raw materials of the pyrazole intermediate disappeared after refluxing for 5h and the temperature was lowered to 10 C, add water 200ml, stirred 0.5h, liquid separation, the organic phase was washed with saturated sodium bicarbonate solution, washed with water, the organic phase was separated, the chloroform was distilled off to obtain fipronil crude. The crude product was recrystallized from toluene to give fipronil 198g, purity 98.5%, the total yield of 81%

Statistics shows that 5-Amino-1-(2,6-dichloro-4-(trifluoromethyl)phenyl)-1H-pyrazole-3-carbonitrile is playing an increasingly important role. we look forward to future research findings about 120068-79-3.