Month: April 2021

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. 400877-57-8, name is Methyl 1-methyl-4-nitro-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below., Recommanded Product: Methyl 1-methyl-4-nitro-1H-pyrazole-3-carboxylate

A solution of 1-methyl-4-nitro-1H-pyrazole-3-carboxylic acid methyl ester (4.8 g, 25.94 mmol) in dry MeOH (100 ml) was thoroughly purged with argon, treated with 10% Pd-C (2.7 g, 2.59 mmol), and again purged with argon. Then the reaction mixture was hydrogenated under a balloon pressure of hydrogen at rt for overnight. The reaction mixture was filtered through a bed of celite. The filtrate was concentrated and dried to give the title compound as gray – whitesolid (3.4 g, 84%), which was used in the next reaction step without further purification.

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 402-61-9, 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. 402-61-9 name is 5-Methyl-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.

23.3 g (0.121 mol) of EDC, 16.4 g (0.121 mol) of HOBt and 26.7 g (0.121 mol) of N’-hydroxy-4-(trifluoromethoxy)benzenecarboximide amide were added successively to a solution of 15.3 g (0.121 mol) of 5-methyl-1H-pyrazole-3-carboxylic acid in 600 ml of anhydrous DMF at RT. The mixture was stirred first at RT for 2 h and then at 140 C. for 5 h. After cooling, the mixture was diluted with 2 litres of water and extracted three times with 1 litre of ethyl acetate each time. The combined organic extracts were washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the solvent was removed on a rotary evaporator. The crude product obtained was purified by means of filtration with suction over a suction filter filled with silica gel (eluent: cyclohexane/ethyl acetate 5:1?1:1). The product fractions were combined and the solvent was removed on a rotary evaporator to such an extent that the product just started to precipitate out. The precipitation was brought to completion at RT. By filtration and further concentration of the mother liquor, two fractions of solid were obtained, which were combined and dried under a high vacuum. 19.7 g (52% of th.) of the title compound were obtained in total in this way.1H-NMR (400 MHz, CDCl3, delta/ppm): 10.75 (broad, 1H), 8.24 (d, 2H), 7.34 (d, 2H), 6.81 (s, 1H), 2.46 (s, 3H).HPLC (method A): Rt=4.72 min.MS (DCI, NH3): m/z=311 [M+H]+.LC/MS (method F, ESIpos): Rt=1.27 min, m/z=311 [M+H]+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-Methyl-1H-pyrazole-3-carboxylic acid, and friends who are interested can also refer to it.

Electric Literature of 127107-23-7, 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. 127107-23-7 name is 1-Methyl-1H-pyrazol-4-amine hydrochloride, 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.

Into a 20 mL round-bottom flask under nitrogen, were placed intermediate 50.3 (83 mg, 0.21 mmol, 1.00 equiv), butan-1-ol (2 mL) and 1-methyl-1H- pyrazol-4-amine hydrochloride (32 mg, 0.39 mmol, 1.20 equiv). The reaction was stirred overnight at 110 C in an oil bath, then concentrated under vacuum. The resulting solution was diluted with 0.5 mL of sodium bicarbonate and concentrated under vacuum. The resulting solution was extracted with DCM/IPA (3/1), and the organic layers were combined and concentrated under vacuum. The crude product was purified using flash column chromatography to furnish 11.4mg (12%) of compound I-SO as a brown solid. LCMS; (ES, m/z): 471 [M+H] ?H NMR (400 MHz, CD3OD): oe 7.828 (s, 1H), 7.526 (s, 1H), 3.842 (s, 3H), 3.6793.710 (m, 4H), 2.5962.626 (m, 4H), 2.216 (s, 3H), 2.0672.082 (d, 2H), 1.3951.460 (m, 13H).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Methyl-1H-pyrazol-4-amine hydrochloride, and friends who are interested can also refer to it.

Electric Literature of 5932-27-4, These common heterocyclic compound, 5932-27-4, name is Ethyl 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.

DMF (40 mL) was added to a flask containing ethyl 1H-pyrazole-3-carboxylate (1.5 g, 10.70 mmol), sodium hydride (0.5 14 g, 12.84 mmol, 60percent dispersion in mineral oil) at 0 °C. After 15 mm at 0 °C, the reaction mixture was allowed to warm up to RT and stirred at RT for 30 mm. The reaction mixture was cooled to 0 °C and a solution of 2-(3-bromopropyl)-2-methyl-1,3- dioxolane (2.69 g, 12.84 mmol), and potassium iodide (0.355 g, 2.141 mmol) in DMF (20 mL)was added. The reaction mixture was stirred at 0 °C for 15 mm, then allowed to warm up to RT and stirred at RT for 16 h. After cooling to 0 °C, the reaction mixture was quenched with aq NH4C1 (30 mL), and all DMF was removed under high vacuum. The residue was diluted withEtOAc (200 mL), washed with brine, dried over Na2SO4, filtered, and concentrated. Flash chromatography (EtOAc/hexanes) afforded Example 113A (0.88 1 g, 3.28 mmol, 31 percent yield) and Example 113B (1.724 g, 6.43 mmol, 60 percent yield). LCMS (ES): m/z 269.10 [M+Hjt Example 113A: 1H NMR (400 MHz, CDC13) oe 7.43 (d, J1.7 Hz, 1H), 6.79 (d, J2.0 Hz, 1H), 4.55 (t,J7.3 Hz, 2H), 4.30 (q,J7.1 Hz, 2H), 3.88 (br d,J=2.9 Hz, 4H), 1.97- 1.84 (m, 2H), 1.71 – 1.57(m, 2H), 1.34 (t,J=7.1 Hz, 3H), 1.26 (s, 3H). Example 113B: 1HNMR(400 MHz, CDC13) oe 7.38(d, J1.7 Hz, 1H), 6.74 (d, J1.7 Hz, 1H), 4.34 (q, J=7. 1 Hz, 2H), 4.17 (br t, J=7.2 Hz, 2H), 3.98-3.69 (m, 4H), 2.02- 1.90 (m, 2H), 1.67- 1.52 (m, 2H), 1.34 (t,J=7.1 Hz, 3H), 1.24 (s, 3H).

The synthetic route of 5932-27-4 has been constantly updated, and we look forward to future research findings.

Reference of 37622-90-5,Some common heterocyclic compound, 37622-90-5, name is Ethyl 4-pyrazolecarboxylate, molecular formula is C6H8N2O2, 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 1: l-(4-Methoxy-benzyl)-lH-pyrazole-4-carboxylic acid ethyl ester [00202] A solution of lH-pyrazole-4-carboxylic acid ethyl ester (0.55 g, 3.95 mmol), 4- methoxybenzyl bromide (0.74 g, 4.74 mmol) and potassium carbonate (1.64 g, 11.9 mmol) in acetone (20 ml) was left to stir at ambient temperature for 16 h then heated at 500C for 1 h. The reaction mixture was allowed to cool to ambient temperature, concentrated under reduced pressure then diluted with water and extracted with dichloromethane (4 x 20 ml). The combined organic phase was washed with saturated ammonium chloride solution (20 ml) and brine (20 ml), dried over anhydrous sodium sulfate, filtered and evaporated. The resultant residue was purified by flash column chromatography on silica (ISCO, 4Og) eluting with pentane on a gradient of ethyl acetate (0-30%). Collecting appropriate fractions afforded the title compound as a colourless oil (1.0 g, 97%). 1H NMR (CDCl3, 300 MHz) 7.92 (s, IH), 7.81 (s, IH), 7.33-7.15 (m, 2H), 6.92-6.86 (m, 2H), 5.23 (s, 2H), 4.26 (q, J = 7.1Hz, 2H), 3.81 (s, 3H), 1.29 (t, J = 7.1Hz, 3H). LCMS (method B): Rtau = 3.27 min, M+H+ = 261.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 4-pyrazolecarboxylate, its application will become more common.

Related Products of 16034-46-1, The chemical industry reduces the impact on the environment during synthesis 16034-46-1, name is 1-Methyl-1H-pyrazole-5-carboxylic acid, I believe this compound will play a more active role in future production and life.

General procedure: The appropriate carboxylic acid (34.2 lmol, 2 eq), EDCIHCl(5.30 mg, 34.2 lmol, 2 eq) and DMAP (17.1 lmol, 1 eq) were combinedin CH2Cl2 (2 mL) and stirred at RT for 10 min. Amine 15(10.0 mg, 17.1 lmol, 1 eq) was added and the resulting mixturestirred at RT overnight. Reaction was, quenched by the additionof saturated aqueous NH4Cl solution (5 mL), extracted with EtOAc(3 5 mL) and the combined organic layers washed with 0.1 Maqueous KOH solution, brine, dried (MgSO4), filtered and concentratedin vacuo.

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, 1-Methyl-1H-pyrazole-5-carboxylic acid, 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. 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, A new synthetic method of this compound is introduced below., HPLC of Formula: C4H4N2O

To a stirred solution of l,3-dibromo-5-isopropoxy-benzene (500 mg, 1.70 mmol) in toluene (15 mL) w’ere added lH-pyrazole-4-carbaldehyde (179.77 mg, 1 87 mmol) and potassium phosphate tribasic anhydrous (722.05 mg, 3.40 mmol) and the reaction was degassed with N?. for 10 minutes. Copper (1) iodide (64.78 mg, 340.16 umol, 1 1.53 uL) and N,N’-dimethyl cyclohexane- 1 ,2-diamine (48.38 mg, 340.16 umol) were added to the reaction and the reaction was again degassed for 10 minutes. The reaction was heated to 130 C for 16 hours in a sealed tube at which point TLC confirmed the formation of product. The reaction was cooled and diluted with water and EtOAc. The organics was separated and aqueous part was extracted with EtOAc. The combined organics was washed with water and brine, dried over Na2S04, and concentrated to afford crude compound that was purified by combi-flash using 20-50% EtOAc in hexane to afford l-(3-bromo-5- isopropoxy-phenyl)-lH-pyrazole-4-carbaldehyde (190 mg, 583.84 umol, 34 33% yield, 95% purity, 000) as brown solid m/z = 309.

The synthetic route of 35344-95-7 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. 834869-10-2, name is Methyl 3-ethyl-1H-pyrazole-5-carboxylate, A new synthetic method of this compound is introduced below., Product Details of 834869-10-2

To a solution of potassium tert-butoxide (1.10 g, 9.8 mmol) in tetrahydrofuran (20 mL) at 23 C. was added 3-ethyl-5-pyrazolecarboxylic acid methyl ester (1.25 g, 8.1 mmol) in tetrahydrofuran (2 mL), followed by 4-(bromomethyl)-2-(trifluoromethyl)pyridine (i.e. the product of Step A, 1.95 g, 8.1 mmol). The reaction mixture was stirred at 23 C. for 4 h and then poured into a 1:1 mixture of water and ethyl acetate (100 mL). The layers were separated and the aqueous layer extracted with ethyl acetate (2×50 mL). The combined organic extracts were washed with brine, dried (MgSO4) and concentrated under reduced pressure. The residue was chromatographed on silica gel, eluting with 0-100% ethyl acetate/hexane to afford the title compound (1.68 g) as a pale yellow oil. [0507] 1H NMR delta 8.66-8.70 (m, 1H), 7.36-7.40 (m, 1H), 7.06-7.13 (m, 1H), 6.73 (s, 1H), 5.46 (s, 2H), 3.94 (s, 3H), 2.48-2.55 (m, 2H), 1.24-1.27 (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.

Reference of 1260243-04-6,Some common heterocyclic compound, 1260243-04-6, name is Ethyl 5-amino-1H-pyrazole-4-carboxylate, molecular formula is C6H9N3O2, 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.

Cs2CO3 (64.20 g, 197.20 mmol) was added to a solution of ethyl 5-amino-1H-pyrazole-4-carboxylate (20.40 g, 131.40 mmol) and ethyl-3-ethoxyacrylate (28.6 mL, 197.20 mmol) in DMF (250 mL). The reaction mixture was stirred at 110 C for 16 h. The mixture was cooled to room temp and the pH was adjusted to 4 by the addition of AcOH (80 mL). The mixture was concentrated in vacuo and the residue partitioned between CH2Cl2/H2O (1000 mL, 1:1). The organic layer was separated and the aqueous layer was extracted with CH2Cl2 (3 X 500 mL). The combined organics were washed with brine, dried (MgSO4) and concentrated. The crude residue was suspended in EtOH (300 mL) and heated to boiling. After cooling to room temperature the solid was collected by filtration, rinsed with EtOH, then Et2O and dried under vacuum to give ethyl 5-oxo-4,5-dihydropyrazolo[1,5-a]pyrimidine-3-carboxylate (25.16 g, 92 %). MS (ESI) calcd for C9H9N3O3 (m/z): 207.06; found: 208 [M+H].

The synthetic route of 1260243-04-6 has been constantly updated, and we look forward to future research findings.

Reference of 4522-35-4, 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. 4522-35-4, name is 3-Iodo-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

INTERMEDIATE 7 Methyl 4-(3 -iodo- 1 H-p yrazol- 1 -yPbenzoate To a solution of 3-iodopyrazole (0.7 g, 3.61 mmol) in DMSO (18.0 mL) was added sodium hydride (60% disp. in oil (0.173 g, 4.33 mmol), and the resulting mixture was stirred for 0.5 h before adding methyl 4- fluoro benzoate (0.556 g, 3.61 mmol). The reaction mixture was stirred at 90 C overnight. The reaction was quenched by the addition of water and extracted with EtOAc. The combined organic extracts were washed with water and brine, dried over MgS04 and concentrated in vacuo. The crude mixture was purified by flash chromatography (ISCO, 40 g, 0-20 % EtOAc in hexanes) to afford methyl 4-(3-iodo-lH-pyrazol-l-yl)benzoate, as a white solid. LCMS calc. – 328.97; found = 328.96 (M+H)+. NMR (500 MHz, CDC13): delta 8.12 (m, 2 H); 7.81 (d, J= 2.4 Hz, 1 H); 7.76 (m, 2 H); 6.65 (m, 1 H); 3.94 (s, 3 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-Iodo-1H-pyrazole, other downstream synthetic routes, hurry up and to see.