Category: 39806-90-1

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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. 39806-90-1

To a solution of 4-iodo-1-methyl-IH-pyrazole (55 gm, 0.264 moles) in N,Ndimethylacetamide (100 ml), potassium ferrocyanide (24.5 gm, 0.058 moles), palladium (II) acetate (0.592 gm, 0.0026 moles)and sodium carbonate (27.98 gm, 0.264 moles) wereadded. The reaction mixture was evacuated and backfihled with nitrogen (3 times). The mixture was stirred for 12 hour at 100-1 10C. Progress of the reaction was monitored by HPLC. The reaction mixture was cooled to 20-30C, to this added Dl water (500 ml), ethyl acetate (500 ml) and stirred for 1 hour at 20-30C. The reaction mixture was filtered through pad of celite. The organic layer was separated and aqueous layer was extracted withethyl acetate (200 ml), stirred for 15 mm and separated the final aqueous layer and organic layer. The organic layer was washed with brine solution (200 ml). Ethyl acetate was recovered at reduced pressure at 60-70C. The mixture was degassed for 2 hour at reduced pressure at 60-70C, cooled the mixture to 20-30C: Hexane (400 ml) was added to the mixture and stirred for 1 hour at 20-30C. The solid product obtained was filtered, washedwith cold Dl water (100 ml) and dried at 40-50C to afford the product, I-Methyl-IHpyrazole-4-carbonitrile.Drywt : 17.94gmYield : 0.32 w/w (63%);

The synthetic route of 39806-90-1 has been constantly updated, and we look forward to future research findings.

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. 39806-90-1 name is 4-Iodo-1-methyl-1H-pyrazole, 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. 39806-90-1

a 1-Methyl-4-phenylethinylpyrazole To a solution of 1-methyl-4-iodopyrazole (208 g, 1 mol) and phenylacetylene (112 g, 1.1 mol) in diisopropylamine (2 l) are added, under nitrogen, copperiodide (2 g), triphenylphosphine (0.1 g) and bis-(triphenylphosphine) palladiumdichloride (0.5 g). The mixture is kept during 3 hours at ca. +35 C. and then heated for 1 hour at +90 C. The cooled reaction mixture is diluted with ethyl acetate and filtrated. Concentration of the filtrate and distillation yields the title compound: b.p. 116-118 C./0.3 mbar, m.p. 70-72 C.

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

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. 39806-90-1 name is 4-Iodo-1-methyl-1H-pyrazole, 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. 39806-90-1

A mixture of 5-((1,2,3,5,6,7-hexahydro-s-indacen-4-yl)amino)-1-((2-(trimethylsilyl)- ethoxy)methyl)-1H-1,2,4-triazole-3-thiol (Intermediate B9) (300 mg, 521.57 mumol, 1 eq), 4-iodo-1-methyl-1H-pyrazole (108 mg, 521.57 mumol, 1 eq), CuI (198 mg, 1.04 mmol, 2 eq) and N,N’-dimethylethane-1,2-diamine (919 mg, 10.43 mmol, 20 eq) in dioxane (4 mL) was stirred at 70C under N2 atmosphere for 2 hours. The reaction mixture was poured into water (10 mL) and extracted with ethyl acetate (3 ¡Á 10 mL). The organic layers were dried over anhydrous Na2SO4, filtered and concentrated in vacuum. The residue was purified by prep-TLC (SiO2, petroleum ether: ethyl acetate, 1:1) to give the title compound (200 mg, 79.44% yield) as a yellow solid.1H NMR (400 MHz, CDCl3) d 7.62 (s, 1H), 7.58 (s, 1H), 6.95 (s, 1H), 6.18 (s, 1H), 5.28 (s, 2H), 3.90 (s, 3H), 3.59 (t, 2H), 2.88 (t, 4H), 2.67 (t, 4H), 2.06-2.03 (m, 4H), 0.96- 0.92 (t, 2H), 0.02 (s, 9H).LCMS: m/z 483.1 (M+H)+(ES+).

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

The chemical industry reduces the impact on the environment during synthesis 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, I believe this compound will play a more active role in future production and life. 39806-90-1

Part B:; The compound 52 (33 mg, 0.08 mmol), 3-iodo-1-methylpyrazole (21 mg, 0.1 mmol), K2CO3 (27 mg, 0.2 mmol), CuI (2 mg, 0.01 mmol) and trans-N, N’-bismethyl-i ,2-cyclohexane diamine (4 muL) were mixed in toluene (3 mL) under Argon. The mixture was sealed under Argon and heated up to 1000C and stirred overnight. After cooling to room temperature, the reaction was worked up and the crude was purified by Prep-LC gave the product 53 (29 mg). HPLC-MS tR = 1.88 min (UV254 nm); mass calculated for formula C25H3IN7O2S 493.2, observed LCMS m/z 494.2 (M+H).

The chemical industry reduces the impact on the environment during synthesis 39806-90-1. I believe this compound will play a more active role in future production and life.

Adding some certain compound to certain chemical reactions, such as: 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, 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 39806-90-1. 39806-90-1

To a solution of intermediate 35.8 (30 mg, 0.097 mmol) in anhydrous l,4-Dioxane (3 mL) was added 4-iodo-l-methyl-lH-pyrazole (40.3 mg, 0.194 mmol), K3PO4 (61.7 mg, 0.291 mmol), (trans)-N, N2-dimethylcy cl ohexane-l, 2-diamine (10 mg, 0.070 mmol) and Cul (5 mg, 0.026 mmol), and the resulting mixture was stirred at 90C under N2 protection for 16 hours. Afterward, the reaction was filtered and concentrated. The crude residue was purified by pre-HPLC (TFA) to give example 35.9, 5-chloro-4-fluoro-l-(l-methyl-lH-pyrazol-4-yl)-6-(l-(oxetan-3-yl)piperidin- 4-yl)-lH-indazole, TFA salt. MS (ESI) m/z calc?d for C19H22CIFN5O [M+H]+ 390, found 390. NMR (500 MHz, CDCI3): d 8.17 (s, 1H), 8.03 (s, 1H), 7.86 (s, 1H), 7.40 (s, 1H), 5.13 (t, .7=7.17 Hz, 2H), 4.81 (m, 2H), 4.18 (m, 1H), 4.03 (s, 3H), 3.59 (m, 2H), 3.43 (m, 1H), 2.78 (m, 2H), 2.46- 2.54 (m, 2H), 2.13 (m, 2H). LRRK2 ICso 6.9 nM.

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 4-Iodo-1-methyl-1H-pyrazole.

39806-90-1, The chemical industry reduces the impact on the environment during synthesis 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, I believe this compound will play a more active role in future production and life.

e-2) Preparation of [0250] [0251] N2 atmosphere. A mixture of intermediate (62) (0.004 mol), 4-iodo-1-methyl-1H-pyrazole (0.0035 mol), 1,4-dioxane (25 ml) and Cs2CO3 (1.6 g) in Xantphos (0.1 g) was degassed. Pd2(dba)3 (0.13 g) was added and the reaction mixture was degassed again. The reaction mixture was stirred at 80-90 C. for 2 hours. After cooling, the reaction mixture was filtered over dicalite. The filtrate was concentrated and the residue was purified on silica gel using DCM/CH3OH (from 100% to 96/4) as eluent. The product fractions were collected and evaporated to dryness. The residue was used as such in the next reaction, yielding 0.14 g of intermediate (64).

The chemical industry reduces the impact on the environment during synthesis 39806-90-1. I believe this compound will play a more active role in future production and life.

39806-90-1, 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. 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, This compound has unique chemical properties. The synthetic route is as follows.

To 4-iodo-1-methyl-1 H-pyrazole (1.0346 g, 4.97 mmol) in THF (20 ml) was added CuI (0.36g, 1.89 mmol), and PdCI2(PPh3J2. The reaction flask was purged with N2 and NEt3 (10.4 ml_, 75 mmol) and ethynyl-trimethyl-silane (5.27 ml, 37 mmol) was added. The reaction mixture was heated at 80 0C overnight for 21 hours. After cooling to room temperature, the reaction was diluted with EtOAc and filtered. The filtrate was washed successively with 1 M HCI, 1 M NaOH and H2O. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography (20:8 v/v petroleum ether : EtOAc to give the product as a brown oil (676 mg).

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.

39806-90-1, Adding some certain compound to certain chemical reactions, such as: 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, 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 39806-90-1.

To a solution of 4-iodo-l-methyl-lH-pyrazole (153 mg, 0.736 mmol) in anhydrous DMSO (15 ml) was added intermediate 20.1-1 (190 mg, 0.613 mmol), (Irans)-N 1.N2-dimethylcyclohexane- 1, 2-diamine (34.9 mg, 0.245 mmol), potassium phosphate (391 mg, 1.840 mmol) and Cul (23.36 mg, 0.123 mmol). The resulting mixture was stirred at 90C under N2 protection for 12 hours. After cooling to room temperature, filtering and concentrating, the crude material was purified by pre-HPLC (TFA) to give example 20.2-1, ( R,R or 5′,5′)-5-chloro-6-(3-nuoro- 1 -(oxetan-3- yl)piperidin-4-yl)-l-(l-methyl-lH-pyrazol-4-yl)-lH-indazole, TFA salt. MS (ESI) m/z calc?d for C19H22CIFN5O [M+H]+ 390, found 390. NMR (400 MHz, CD3OD) d 8.17 (s, 2H), 7.96 (s, 1H), 7.88 (s, 1H), 7.65 (s, 1H), 5.16-5.41 (m, 1H), 4.76-4.86 (m, 4H), 4.36 (q, J = 6.36 Hz, 1H), 4.01 (s, 3H), 3.69-3.85 (m, 2H), 3.41 (m, 1H), 2.85-3.03 (m, 2H), 2.27 (m, 1H), 1.95-2.11 (m, 1H). LRRK2 IC50 1.7 nM.

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 39806-90-1.

39806-90-1, Adding a certain compound to certain chemical reactions, such as: 39806-90-1, name is 4-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 39806-90-1.

General procedure: 4-Iodo-1-methyl-1H-pyrazole 1 (101 mg, 0.5 mmol) and phenylboronic 2 (59 mg, 0.5 mmol) were dissolved in DME (3 mL) and H2O (1.2 mL) in a microwave vial under a nitrogen atmosphere. Pd(PPh3)4 (2 mmol%, 11.6 mg) and Cs2CO3 (407.3 mg, 1.25 mmol) were added, and the reaction mixture was irradiated in a microwave apparatus at 90 C for 5-12 min. After the reaction mixture was cooled to ambient temperature, the product was concentrated, and the crude mixture was purified by silica gel column chromatography using petroleum ether/acetone as eluent to give the title compound.

According to the analysis of related databases, 39806-90-1, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 39806-90-1, name is 4-Iodo-1-methyl-1H-pyrazole, 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. 39806-90-1

General procedure: 4-Iodo-1-methyl-1H-pyrazole 1 (101 mg, 0.5 mmol) and phenylboronic 2 (59 mg, 0.5 mmol) were dissolved in DME (3 mL) and H2O (1.2 mL) in a microwave vial under a nitrogen atmosphere. Pd(PPh3)4 (2 mmol%, 11.6 mg) and Cs2CO3 (407.3 mg, 1.25 mmol) were added, and the reaction mixture was irradiated in a microwave apparatus at 90 C for 5-12 min. After the reaction mixture was cooled to ambient temperature, the product was concentrated, and the crude mixture was purified by silica gel column chromatography using petroleum ether/acetone as eluent to give the title compound.

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 39806-90-1.