Tag: M.W:200-300

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. 1353100-91-0, name is Ethyl 3-bromo-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Product Details of 1353100-91-0

To a solution of NaH (275 mg, 6.86 mmol, 60% purity) in THF (5 mL) was added dropwise a solution of ethyl 3-bromo-lH-pyrazole-4-carboxylate (1.0 g, 4.57 mmol) in THF (10 mL) at 0 C. After addition, the mixture was stirred at this temperature for lh, and then Mel (2.93 g, 20.64 mmol, 1.29 mL) was added dropwise at 0 C. The resulting mixture was stirred at 25 C for 19h. The reaction mixture was quenched by addition sat. H4CI (5 mL), and then diluted with H20 (10 mL) and extracted with EtOAc (20 mL x 2). The combined organic layers were washed with brine (15 mL x 2), dried over Na2S04, filtered and concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (Si02, Petroleum ether/Ethyl acetate = 8/1 to 5: 1) to give the Compound 142A (120 mg, yield: 11.27%) was obtained as a yellow oil and Compound 142B (370.00 mg, yield: 34.74%) was obtained as a white solid. (1387) [0574] 1H NMR (400MHz, CDC13) (142A) delta 7.93 (s, 1H), 4.42 – 4.21 (m, 2H), 3.97 – 3.82 (m, 3H), 1.36 (t, J = 7.2 Hz, 3H) (1388) [0575] 1H NMR (400MHz, CDC13) (142B) delta 7.83 (s, 1H), 4.30 (q, J = 7.0 Hz, 2H), 3.94 – 3.86 (m, 3H), 1.41 – 1.28 (m, 3H).

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.

Application of 866837-96-9, 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. 866837-96-9, name is Ethyl 5-amino-1-phenyl-1H-pyrazole-3-carboxylate belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Ethyl 5-amino-1-phenyl-1H-pyrazole-3-carboxylate (498 mg) synthesized according to the method described in W02004/98589 and 4-dimethylaminopyridine (21 mg) were dissolved in pyridine (10 mL), and benzenesulfonyl chloride (461 mg) was added at room temperature. After stirring at 85C for 8 hr, 1 mol/L hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The extract was washed with 1 mol/L hydrochloric acid, water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate=1:1?ethyl acetate), and the obtained solid was washed with a mixed solvent of diisopropyl ether and ethyl acetate to give the title compound as a brown powder (yield 445 mg, yield 69%). 1H-NMR(CDCl3)delta:1.40(3H,t,J=7.2Hz), 4.40(2H,q,J=7.2Hz), 5.29(1H,s), 6.79(1H,s), 7.07-7.10(2H,m), 7.35-7.49(5H,m), 7.60-7.65(1H,m), 7.68-7.72(2H,m).

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, Ethyl 5-amino-1-phenyl-1H-pyrazole-3-carboxylate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 285984-25-0,Some common heterocyclic compound, 285984-25-0, name is 3-(tert-Butyl)-1-(p-tolyl)-1H-pyrazol-5-amine, molecular formula is C14H19N3, 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.

In a 250 mL round botom flask, 100 mL of ethanol was added, (30 mmol) of pivaloylacetonitrile, (33.63 mmol) of 4-methylphenylhydrazine, A solution of 3.6 mL of concentrated hydrochloric acid was added dropwise with stirring,Heated to reflux for 8 hours, cool down, concentrate, The residue was adjusted to pH 10-11 with dilute sodium hydroxide, Extracted three times with ethyl acetate, Dried over anhydrous sodium sulfate, concentrate, The resulting solid was recrystallized from ethyl acetate / petroleum ether to give white crystals C, Yield 80.3%. 5-tert-butyl-2-p-methylphenyl-3-aminopyrazole (3.5 mmolC) was placed in a 100 ml three-Dissolved in 30 ml of tetrahydrofuran, Place the three-necked flask in a cryogenic tank to cool to -20 C, 2.9 g of sodium bicarbonate was added in portions with stirring, After 15 min, A solution of trichloroethyl chloroformate (3.5 mmol) was added dropwise, Control the solution temperature does not exceed 0 deg C, After dripping, Continue stirring for 30min, And then heated to 0 C for 12 h. After completion of the reaction, The mixture is filtered, The residue was washed with ethyl acetate, The filtrate was concentrated, Yield 85%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(tert-Butyl)-1-(p-tolyl)-1H-pyrazol-5-amine, its application will become more common.

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. 37687-24-4, name is Diethyl 3,5-pyrazoledicarboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: Diethyl 3,5-pyrazoledicarboxylate

NaOH (3.53 g, 88 mmol) was added to a solution of diethyl 1H-pyrazole-3,5- dicarboxylate (5.35 g, 25.2 mmol) in acetonitrile (40 mL). After 30 mi 2- chloroethanamine hydrochloride (3.22 g, 27.7 mmol) and tetrabutylammonium hydrogen sulfate (0.43 g, 1.26 mmol) were added. The mixture was refluxed for 20 h. Aftercooled, conc. HC1 (5 mL) was added. The mixture was extracted with CH2C12, washed with brine. The combined organic layers were dried over Na2SO4, filtered and concentrated. Normal phase chromatography afforded Intermediate 138 (2.72 g, 52%) as a white solid. ?H NMR (500MHz, DMSO-d6) oe 8.39 (br s, 1H), 7.07 (s, 1H), 4.40 (dd, J6.7, 5.5 Hz, 2H), 4.27 (q, J7.2 Hz, 2H), 3.68 – 3.61 (m, 2H), 1.28 (t, J=7.0 Hz, 3H).LC-MS(ESI) m/z: 210.1 [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.

Adding a certain compound to certain chemical reactions, such as: 155600-99-0, name is 3,5-Dibromo-1-methyl-4-nitro-1H-pyrazole, 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 155600-99-0, SDS of cas: 155600-99-0

Production example 8 3-bromo-5-tert-butylamino-1-methyl-4-nitropyrazole 1.5 g (5.26 mmoles) of 3,5-dibromo-1-methyl-4-nitropyrazole are heated in a solution of 20 ml tert-butylamine in 30 ml ethanol for 20 hours at boiling temperature. After cooling, the reaction mixture is poured on 150 ml water, the separated product is filtered and washed with 100 ml water. After vacuum drying, 1.14 g (78 percent of theory) of 3-bromo-5-tert-butylamino-1-methyl-4-nitropyrazole are obtained in the form of pale yellow flakes with a melting point of 75 to 77 C. 1 H-NMR (60 MHz, DMSO-d6):=5.35 (s; 1H; –NH; exchanges with D2 O), 3.75 (s; 3H; N–CH3) and 1.20 ppm (s; 9H; –C(CH3)3). MS (70 eV): m/e=277 (M+).

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

Some common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, 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. category: pyrazoles-derivatives

3 -Difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid ethyl ester (53.3 mg) was dissolved in liquid ammonia (10 mL). A column (500mm x 4.6mm i.d.) packed with aluminium oxide (4.501 g) was placed in the oven and the temperature was raised to 100C before pure liquid ammonia was pumped through. Then pure liquid ammonia was pumped through the system at 0.3 mLmin”1 and the pressure adjusted to 100 bar using an adjustable back pressure regulator.The system was left pumping pure liquid ammonia for 10 minutes then switched to the reaction solution at 0.3mL min^forSO min. At this time, pure liquid ammonia was pumped through the system for another 1 hour at 0.3mL min”1. All the reaction solution was collected as it exited the reaction column, at the end of the reaction, the ammonia was allowed to evaporate, the residue was dissolved in methanol and analysed by HPLC (87-91% conversion, 98.4% selectivity).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 141573-95-7, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 92525-10-5, name is 3-Iodo-1-methyl-1H-pyrazole, 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 92525-10-5, name: 3-Iodo-1-methyl-1H-pyrazole

Into a 50-mL vial purged and maintained with an inert atmosphere of nitrogen, 3- iodo-1-methyl-1H-pyrazole (500 mg, 2.40 mmol) was dissolved in acetonitrile (10 mL). Then methyl prop-2-enoate (2.07 g, 24.03 mmol), palladium diacetate (108 mg, 0.48 mmol), tri-ortho- tolylphosphine (292 mg, 0.96 mmol) and triethylamine (1.216 g, 12.02 mmol) were added. The resulting solution was stirred for 2 h at 80oC under nitrogen atmosphere. The reaction mixture was cooled and concentrated under vacuum. The residue was subjected to purification by FCC eluting with ethyl acetate/petroleum ether (1:1). This afforded the title compound (130 mg, 33%) as a yellow oil. MS: (ES, m/z): 167[M+H]+.

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Application of 73387-46-9,Some common heterocyclic compound, 73387-46-9, name is 3-(4-Bromophenyl)-1H-pyrazole, molecular formula is C9H7BrN2, 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.

Intermediate A4 6-methoxy-2-(4-( 1 -methyl- 1 H-pyrazol-3 -yl)phenyl)-3.4-dihydroisoquinolin- 1 (2H)-one and 6-methoxy-2-(4-(l -methyl- lH-pyrazol-5-yl)phenyl)-3.4-dihydroisoquinolin-l(2H)-one Step 1 : 3-(4-bromophenyl)-lH-pyrazole (0.377 g, 1.690 mmol) was dissolved in THF (8.45 ml). 60% Sodium hydride in oil (0.101 g, 2.54 mmol) was added and the reaction was stirred at rt for 15 min. Methyl iodide (0.116 ml, 1.859 mmol) was added and the reaction was stirred overnight at room temperature. The reaction was quenched with water and extracted three times with dichloromethane. The organic layers were combined, passed through a phase separator and concentrated. The crude material was purified via silica gel chromatography using 0-50% ethyl acetate in heptanes to afford a 2: 1 mixture of products (370 mg, 1.561 mmol, 92 % yield) as a yellow solid. NMR (400 MHz, CHLOROFORM-^ delta ppm 3.86 – 3.95 (m, 3 H), 3.97 (s, 6 H), 6.34 (d, J=1.52 Hz, 1 H), 6.54 (d, J=2.02 Hz, 2 H), 7.30 – 7.33 (m, 2 H), 7.40 (d, J=2.53 Hz, 2 H), 7.49 – 7.56 (m, 5 H), 7.59 – 7.64 (m, 2 H), 7.66 – 7.72 (m, 4 H). LC MS (m/z, MH+): 238.9.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-(4-Bromophenyl)-1H-pyrazole, its application will become more common.

Adding a certain compound to certain chemical reactions, such as: 285984-25-0, name is 3-(tert-Butyl)-1-(p-tolyl)-1H-pyrazol-5-amine, 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 285984-25-0, Application In Synthesis of 3-(tert-Butyl)-1-(p-tolyl)-1H-pyrazol-5-amine

General procedure: A solution of compounds 10a-d or compounds 17a-d (1.0 mmol) in dichloromethane (10 mL) was slowly added to a stirred solution of triphosgene (109 mg, 0.36 mmol) in dichloromethane (50 mL) over a period of 30 min using a syringe. After stirring for a further 30 min, a solution of compound 25a-r (0.6 mmol) and triethylamine (0.4 mL, 2.77 mmol) in dichloromethane (10 mL) was added in one portion. The reaction mixture was stirred for 2 h at room temperature. After completion of the reaction, the reaction was poured into water (50 mL) and extracted three times with dichloromethane. The organic layer was washed with water (5 mL), sat. NaCl solution (5 mL), anddried over Na2SO4. After evaporation of solvent under vacuum, the residue was purified by silica gel chromatography to give the desired chromanylurea or 2H-chromenyl urea compounds.

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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. 706819-66-1, name is 2-Bromo-1-(1-methyl-1H-pyrazol-4-yl)ethanone, A new synthetic method of this compound is introduced below., Formula: C6H7BrN2O

General procedure: A 40 mL vial was charged with 5e (640 mg, 1.61 mmol), 12 (546 mg, 1.77 mmol), anhydrous MeCN (15mL) and -325 mesh K2CO3 powder (266 mg, 1.93 mmol). The mixture was stirred at 20 C for 18 h, before being diluted with EtOAc (15 mL) and H2O (15 mL). The phases were separated and the aqueous phase was extracted with additional EtOAc (2 x 10mL). The combined extracts were dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica (heptane – EtOAc) to afford 520 mg (52%) of 15d and 410 mg (41%) of 16d.

The synthetic route of 706819-66-1 has been constantly updated, and we look forward to future research findings.