Tag: M.W:100-200

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.

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.

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.

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.

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.

Adding a certain compound to certain chemical reactions, such as: 3112-31-0, name is 1H-Pyrazole-3,5-dicarboxylic acid, 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 3112-31-0, Product Details of 3112-31-0

(2R,4R)-4-Amino-5-biphenyl-4-yl-2-hydroxypentanoic acid butyl ester (HCl salt; 108 mg, 286 mummol, 1.0 eq.), 3,5-pyrazoledicarboxylic acid (66.9 mg, 429 mumol, 1.5 eq.), and HATU (160 mg, 430 mumol, 1.5 eq.) were combined in DMF (5 mL), and the resulting mixture was stirred for 2 minutes. DIPEA (150 muL) was added and the mixture was stirred for 1 hour. The mixture was dried under vacuum, and the product was purified using reverse phase chromatography to yield the title compound as a TFA salt (60 mg; purity 98percent). MS m/z [M+H]+ calc’d for C26H29N3O6, 480.21. found 480.4).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference of 2458-26-6, The chemical industry reduces the impact on the environment during synthesis 2458-26-6, name is 3-Phenyl-1H-pyrazole, I believe this compound will play a more active role in future production and life.

EXAMPLE 154; Step 1; 1-(4-Methoxy-benzyl)-3-phenyl-1H-pyrazole; A mixture of 3-phenyl-1H-pyrazole (1.35 g, 9.36 mmol), 4-methoxybenzyl chloride (1.5 g, 9.7 mmol) and K2CO3 (3.3 g, 24.2 mmol) in methyl ethyl ketone was refluxed for 24 h. The salts were filtered off, and the solvent was removed in vacuo. The residue was purified by a column chromatography on silica gel to yield the title compound (2.2 g, 89%).

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-Phenyl-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

Synthetic Route of 632365-54-9, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 632365-54-9, name is Methyl 5-amino-1H-pyrazole-3-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Under argon, lithium borohydride (2M in THF, 84.2 ml) was added dropwise to a stirred solution of methyl 5-aminopyrazole-3-carboxylate (9.5 g) in tetrahydrofuran (300 ml). The resultant mixture was heated to reflux for 16 hours. The mixture was cooled and methanol was added dropwise to quench residual reducing agent. The mixture was evaporated. Methanol (200 ml) was added to the residue and insoluble salts were removed by filtration. The filtrate was evaporated and the residue was purified by column chromatography on silica using a solvent gradient of 9:1 to 4:1 of methylene chloride and methanol as eluent. There was thus obtained 3-amino-5-hydroxymethyl-li?-pyrazole (5.6 g) 1H NMR: (DMSOd6) 4.27 (s, 2H)5 4.3-5.2 (2 br s, 3H), 5.29 (s, IH).

The chemical industry reduces the impact on the environment during synthesis Methyl 5-amino-1H-pyrazole-3-carboxylate. I believe this compound will play a more active role in future production and life.

These common heterocyclic compound, 5203-77-0, name is 1,3-Dimethyl-1H-pyrazol-5-ol, 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. COA of Formula: C5H8N2O

At room temperature, add 1,3-dimethyl-1H-pyrazole-5-ol (1.12 g, 0.01 mol),(3.95 g, 0.05 mol) pyridine was sequentially dissolved in 20 ml of dichloromethane. The low temperature bath was cooled to 3 C.To the above mixture, 7-chloro-3-(methylsulfonyl)quinoline-8-carbonyl chloride (6.08 g, 0.02 mol) was added dropwise at a dropping rate of 2 drops per 30 seconds.After the dropwise addition was completed, the mixture was naturally warmed to room temperature and reacted for 5 hours. To the reaction mixture was added 10 ml of a saturated aqueous sodium hydrogen carbonate solution, and dichloromethane (3 * 15 ml) was extracted. The organic layers were combined, washed with water (1 * 15 ml), washed with saturated brine, and dried over anhydrous magnesium sulfate.The product was desolvated under reduced pressure to obtain 3.03 g of the product with a yield of 80%.

The synthetic route of 1,3-Dimethyl-1H-pyrazol-5-ol has been constantly updated, and we look forward to future research findings.

Related Products of 25016-12-0, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 25016-12-0, name is 1,3-Dimethyl-1H-pyrazole-4-carbaldehyde, This compound has unique chemical properties. The synthetic route is as follows.

To a solution of 3′-chloro-3,4,5,6-tetrahydro-2H-[l,2′]bipyrazinyl (3 g, 15.1 mmol, 1 eq) and l,3-dimethyl-lH-pyrazole-4-carbaldehyde (2.0 g, 16.6 mmol, 1.1 eq) in DCE (75 mL) add sodium triacetoxyborohydride (4.8 g, 22.6 mmol, 1.5 eq) and stir at room temperature over the weekend. Add 2 N sodium hydroxide (100 mL), separate the layers, extract the aqueous layer twice with DCM (75 mL), dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 0: 100 to 10:90 –65-methanol:DCM). Combine only the fractions which contain the main component and concentrate to give the title preparation as a viscous yellow oil (2.14 g, 46%). Combine all other fractions which contain main component plus impurities, concentrate then repeat the chromatography step to recover further material (1.6 g, 35%, total yield 81%). MS (ES): m/z = 307.1 [M+H]+.

The chemical industry reduces the impact on the environment during synthesis 1,3-Dimethyl-1H-pyrazole-4-carbaldehyde. I believe this compound will play a more active role in future production and life.