Tag: M.W=0-100

288-13-1,Some common heterocyclic compound, 288-13-1, name is 1H-Pyrazole, molecular formula is C3H4N2, 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: Complex 2 (0.05 mmol) was added to a 5 mL of a sealed tube containing the aryl iodide or bromide (0.5 mmol), 1H-pyrazole (0.75 mmol), NaOH (1 mmol), and DMSO (1 mL). The mixture was stirred at 100 C for 12 h. After being cooled to room temperature, the mixture was quenched with 10 mL H2O and extracted with EtOAc(3 ¡Á 20 mL). The combined EtOAc extracts were dried with anhydrous Na2SO4, filtered and the solvent was removed under reduced pressure.The residue was purified by flash column chromatography on silicagel with PE/EtOAc (from 10:1 to 5:1) as the eluent to afford the pure products. All N-aryl pyrazoles reported here are known products and were characterised by 1H NMR, and GC-MS.

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

35277-02-2, 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 35277-02-2 as follows.

[0129] To a solution of 2-bromo-1-[4-methylphenyl]propan-1-one (IV-2) (commercially available, purity 90%, 1.60 g, 6.34 mmol) in acetonitrile (45 mL) was added successively anhydrous potassium carbonate (1.05 g, 7.61 mmol) and 4-fluoro-1H-pyrazole (546 mg, 6.34 mmol). After stirring at room temperature overnight, the reaction mixture was filtered and concentrated under reduced pressure.Purification of the residue by flash chromatography on silica (cyclohexane/ethyl acetate, 98/2 to 70/3 0) provided 2-(4-fluoro- 1 H-pyrazol- 1 -yl)- 1- [4-methylphenyl]propan- 1-one (v-2) (purity 98%, 1.37 g, 91%). ?H NMR (400 MHz, DMSO-d6) 1.60 (d, 3H), 2.37 (s, 3H), 6.14 (q, 1H), 7.33 (d, 2H), 7.44 (d, 1H), 7.87 (d, 2H), 8.06 (d, 1H).

According to the analysis of related databases, 4-Fluoro-1H-pyrazole, the application of this compound in the production field has become more and more popular.

35277-02-2, Name is 4-Fluoro-1H-pyrazole, 35277-02-2, 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.

To a solution of [3-[2-(9-cyano-3,5- dihydro-2H-pyrido[3,4-f][l,4]oxazepin-4-yl)-l,l-dimethyl-2-oxo-ethyl]cyclobutyl] methanesulfonate (200 mg, 0.51 mmol) and 4-fluoro-lH-pyrazole (88 mg, 1.02 mmol) in DMF (2 mL) was added CS2CO3 (331 mg, 1.02 mmol) at 25 C, and then the solution was stirred at 100 C for 12 h. The reaction mixture was partitioned between DCM/i-PrOH (v:v = 3 : 1, 3 x 10 mL) and water (5 mL). The organic phase was separated, washed with brine (5 mL), dried over anhydrous Na2S04, filtered and concentrated under reduced pressure. The residue was purified by prep-HPLC with the following conditions: column: Xtimate C18 150 25 mm 5 muiotaeta; mobile phase: [water (10 mM H4HC03)-ACN]; B%: 30%-50% over 10.5 min. to provide the title compound as a light yellow oil. LCMS: m/z = 384.4 [M+H]+.

Statistics shows that 4-Fluoro-1H-pyrazole is playing an increasingly important role. we look forward to future research findings about 35277-02-2.

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 35277-02-2 as follows. 35277-02-2

(5)-3-(4-Fluoro- lH-pyrazol- l-yl)-2-hydroxy-2-methyl-N-(4-nitro-3-(trifluoromethyl)phenyl)- propanamide (C14H12F4N4O4) (1046) (0902) 1046 [00415] To a dry, nitrogen-purged 100 mL round-bottom flask equipped with a dropping funnel under argon atmosphere containing 4-fluoro-lH-pyrazole (691 mg, 8.03 mmol), NaH of 60% dispersion in mineral oil (674 mg, 16.9 mmol) was added in 60 mL of anhydrous THF solvent at ice- water bath. The mixture was stirred 30 min at the ice- water bath. Into the flask through dropping funnel, a solution of ( ?)-3-bromo-2-hydroxy-2-methyl-N-(4-nitro-3-(trifluoromethyl)phenyl)propanamide (2.98 g, 8.03 mmol) in 10 mL of anhydrous THF was added under argon atmosphere at the ice-water bath, and stirred overnight at RT. After adding 1 mL of H2O, the reaction mixture was condensed under reduced pressure, and then dispersed into 50 mL of EtOAc, washed with 50 mL (x 2) water, evaporated, dried over anhydrous MgS04, and evaporated to dryness. The mixture was purified with flash column chromatography using as an eluent EtOAc/hexane in a 1:2 ratio to produce the titled compound (2.01 g, 67%) as yellow solid. (0903) [00416] Compound 1046 was characterized as follows: NMR (400 MHz, CDC13) delta 9.14 (bs, 1H, NH), 8.01 (s, 1Eta), 7.97-7.91 (m, 2Eta), 7.38 (d, = 3.6 Hz, 1H), 7.35 (d, = 4.4 Hz, 1H), 5.95 (s, 1H, OH), 4.56 (d, = 14.0 Hz, 1H), 4.17 (d, = 14.0 Hz, 1H), 1.48 (s, 3H); 19F NMR (CDCI3 decoupled) delta -60.13, -176.47; MS (ESI) mJz 375.08 [M – H] ~; 377.22 [M + H] +; 399.04 [M + Na] +.

According to the analysis of related databases, 35277-02-2, the application of this compound in the production field has become more and more popular.

The chemical industry reduces the impact on the environment during synthesis 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, I believe this compound will play a more active role in future production and life. 35344-95-7

General procedure: To a stirred solution of 1H-pyrazole-4-carbaldehyde (1.00 g. 10.4 mmoi) and6-bromo-4-rnethyinicotinonitrile (2.05 g, 10.4 mrnol) in dioxane (15 mL) were added K2C03 (4.31 g, 31.2 mrnol) The resulting reaction mixture was degassed with nitrogen for 5 minutes and was added copper(1) iodide (0595 g, 3. 12 mmoi), followed by trans_N,NLdimethylcyciohexanei .2-diamine (2.59 mL, 16.4 mmoi). The resulting reaction mixture was degassed with nitrogen for an additional 5 minutes and heated at110 ¡ãC for 1 h under microwave irradiation. The reaction mixture was cooled to ambient temperature, filtered through celite and the organic layer was concentrated under reduced pressure. The residue was purified by column chromatography (Redisep-24 g, 20-40percent EtOAc/ n-hexane) to obtain Intermediate 9 (115 g, 52.1percent) as a pale yellow solid. ?H NMR (300 MHz, DMSO?d6) oe ppm 2.62 (s, 3 H), 8.10 (s, I Fl), 8.38 (s, I H), 8.95 (s, IH), 9.37 (s, I H), 998 (s, I H). LCMS (method-i)), retention time 1.68 mi [M+Hi213.2.

The chemical industry reduces the impact on the environment during synthesis 35344-95-7. I believe this compound will play a more active role in future production and life.

3920-50-1, Adding some certain compound to certain chemical reactions, such as: 3920-50-1, name is Pyrazole-3-carboxaldehyde, 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 3920-50-1.

Reference Example 11-1 1 1-Allyl-1H-pyrazole-5-carbaldehyde Pyrazole-3-carbaldehyde (3.00 g, 31.2 mmol) was dissolved in DMF (20 ml), and thereto were added potassium carbonate (6.47 g, 46.8 mmol) and allyl bromide (3.50 g, 32.8 mmol) with stirring. The mixture was stirred at room temperature for 6 hours, and thereto was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography to give the title compound (429 mg, 10 percent). 1H NMR (CDCl3, 400 MHz) delta 9.86 (s, 1H), 7.59 (d, 1H, J = 2.0 Hz), 6.93 (d, 1H, J = 2.0 Hz), 6.04 – 5.94 (ddt, 1H, J = 10.3, 17.1, 5.7 Hz), 5.19 (dd, 1H, J = 1.2, 10.3 Hz), 5.16 (d, 2H, J = 5.7 Hz), 5.09 (dd, 1H, J = 1.2, 17.1Hz).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 3920-50-1.

A common compound: 28466-26-4, name is 4-Aminopyrazole, 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. 28466-26-4

10054] A 250-mE 3-neck flask was charged with 1H-pyra- zol-4-amine (5 g, 60.2 mmol) and dichioromethane (50 mE). The resulting suspension was cooled to 5 C. and triethylamine (9.13 g, 90.0 mmol) was added, followed by acetic anhydride (7.37 g, 72.2 mmol) at <20 C. The reaction was stirred at room temperature for 18 hours, at which point thin layer chromatography [Eluent: ethyl acetate] analysis indicated that the reaction was incomplete. Additional triethylamine (4.57 g, 45.0 mmol) and acetic anhydride (3.70 g, 36.0 mmol) were added and the reaction was heated at 30 C. for an additional 3 hours to give a dark solution, at which point thin layer chromatography analysis indicated that only a trace of starting material remained. The reaction mixture was purified by flash column chromatography using ethyl acetate as eluent. The fractions containing pure product were combined and concentrated to dryness to afford an off-white solid. The solid was dried under vacuum at room temperature for 18 hours (5.55 g, 55%): ?H NMR (400 MHz, DMSO-d5) oe 10.30 (s, 1H), 8.39 (d, J=0.7 Hz, 1H), 7.83 (d, J=0.7 Hz, 1H), 2.60 (s, 3H), 2.03 (s, 3H); ElMS mlz 167 ([M]j. 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, 28466-26-4, other downstream synthetic routes, hurry up and to see.

25222-43-9, A common compound: 25222-43-9, name is (1H-Pyrazol-4-yl)methanol, 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.

A mixture of (5S,7S)-2-bromo-7-fluoro-5-phenyl-6,7-dihydro-5H-pyrrolo[l,2-b] [l,2,4]triazole (300 mg, 1.06 mmol), copper(l) iodide (1064 mg, 10.63 mmol), (lSSj-N lS -dimethylcyclohexane-l- diamine (1210 mg, 8.51 mmol), cesium carbonate (1039 mg, 3.19 mmol) and (lH-pyrazol-4- yl)methanol (1064 mg, 10.63 mmol) in 1,4-dioxane (2.5 mL) was heated at 140 ¡ãC for 3h a sealed tube under microwave. After cooled, the mixture was diluted with water (30 mL) and extracted with ethyl acetate (3 x 15 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography (silica gel, 100-200 mesh, 0 to 15percent MeOH in isopropyl acetate) to afford final product (169 mg, 53percent) as a white solid. LC-MS T = 0.92 min, m/z = 300.1 (M+H) +. LCMS (5 to 95percent acetonitrile in water + 0.1percent formic acid over 2 mins) retention time 0.92 min, ESI+ found [M+H] = 300.1

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, (1H-Pyrazol-4-yl)methanol, other downstream synthetic routes, hurry up and to see.

288-13-1, 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. 288-13-1, name is 1H-Pyrazole, A new synthetic method of this compound is introduced below.

The acetic anhydride and fuming nitric acid are slowly mixed in an ice water bath at a volume ratio of 5.5:1 to obtain a nitrating agent, and the nitratingagent and the pyrazole acetic acid solution are respectively delivered to the microchannel reactor through a high-pressure constant-flow pump with precise flow control. The twoinlets control the molar ratio of nitric acid to pyrazole to be 1.1:1. At 45-70 ¡ãC, the two liquids are instantaneously mixed in the microchannel reactorand reacted. The reaction solution is poured into crushed ice and filtered. It was washed with ice water and dried under vacuum to give N-nitropyrazole; theflow rate of the acetic acid solution of the pyrazole was 0.1 mL/min.The yield and purity of N-nitropyrazole are shown in Table 1 and Figure 2.

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