Category: 3469-69-0

Related Products of 3469-69-0, These common heterocyclic compound, 3469-69-0, name is 4-Iodopyrazole, 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.

General procedure: To a solution of pyrazole 1-13 (1 equiv.) and trifluoroacetic acid (0.01 equiv.) in dichloromethane(for 1 mol of pyrazole – 1 L of dichloromethane were used) ethyl vinyl ether (1.27 equiv.) wasadded dropwise, keeping the temperature between 28-32 C (exothermic reaction) and left to stir atroom temperature for 12-78 hours. Dichloromethane was washed with saturated NaHCO3 solution(1 × 250 mL – for 1 L of dichloromethane) then with deionized H2O (1 × 250 mL). Organic layerwas dried with anhydrous Na2SO4, and evaporated under reduced pressure. Products were purifiedby distillation or recrystallization.

Statistics shows that 4-Iodopyrazole is playing an increasingly important role. we look forward to future research findings about 3469-69-0.

3469-69-0, name is 4-Iodopyrazole, 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. Application In Synthesis of 4-Iodopyrazole

1-Methyl-4-iodopyrazole (18) 4-Iodopyrazole (1) (5.0 g 25.7 mmole) was dissolved in DMF (50 mL), potassium carbonate (4.26 g 30.9 mmole) was added and stirred (2 mins) before iodomethane (1.76 mL, 4.01 g 28.3 mmole) was added. The reaction was stirred rapidly at r.t. for 17 hrs. It was filtered through a Celite pad. The filtrate was evaporated to a small volume, about 10 mL, using a rotary evaporator with a high vac. pump and the water bath at 60 C. Water (120 mL) was added to the residue. The filtered solids on the Celite pad were washed with ethyl acetate (50 ml) and these washings were used to extract the product from the aqueous. The aqueous was extracted with more ethyl acetate (2*50 mL). The combined organics were washed with water (3*30 mL) and with brine; dried and evaporated to give the title compound as a solid 4.56 g, 85%. 1H-NMR (CDCl3, 500 MHz): delta 3.93 (s, 3H) 7.42 (s, 1H), 7.50 (s, 1H).

The synthetic route of 3469-69-0 has been constantly updated, and we look forward to future research findings.

Reference of 3469-69-0, These common heterocyclic compound, 3469-69-0, name is 4-Iodopyrazole, 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.

Under the protection of nitrogen, the 4-iodo -1H-pyrazole (3.88g, 20mmol) dissolved in DMF (50 ml) in, cooling to 0 C, adding NaH (1.66g, 55 . 33mmol, in 80% dispersion in mineral oil), mixture in 0 C stirring 10 minutes, to continue to slowly adding the CH 3 I (2.5 ml, 38 . 76mmol). Reaction solution stirring the mixture at room temperature for 22 hours later, water (100 ml) quenching, and using EtOAc (200 ml) extraction. Organic phase Na 2 SO 4 drying, concentrating under reduced pressure, to obtain the title compound as a buff solid (3.99g, 95.9%).

The synthetic route of 3469-69-0 has been constantly updated, and we look forward to future research findings.

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. 3469-69-0, name is 4-Iodopyrazole, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C3H3IN2

1-Methyl-4-iodopyrazole (18) 4-Iodopyrazole (1) (5.0 g 25.7 mmole) was dissolved in DMF (50 mL), potassium carbonate (4.26 g 30.9 mmole) was added and stirred (2 mins) before iodomethane (1.76 mL, 4.01 g 28.3 mmole) was added. The reaction was stirred rapidly at r.t. for 17 hrs. It was filtered through a Celite pad. The filtrate was evaporated to a small volume, about 10 mL, using a rotary evaporator with a high vac. pump and the water bath at 60 C. Water (120 mL) was added to the residue. The filtered solids on the Celite pad were washed with ethyl acetate (50 ml) and these washings were used to extract the product from the aqueous. The aqueous was extracted with more ethyl acetate (2*50 mL). The combined organics were washed with water (3*30 mL) and with brine; dried and evaporated to give the title compound as a solid 4.56 g, 85%. 1H-NMR (CDCl3, 500 MHz): delta 3.93 (s, 3H) 7.42 (s, 1H), 7.50 (s, 1H).

According to the analysis of related databases, 3469-69-0, the application of this compound in the production field has become more and more popular.

Adding a certain compound to certain chemical reactions, such as: 3469-69-0, name is 4-Iodopyrazole, 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 3469-69-0, Recommanded Product: 3469-69-0

Diisopropylethylamine (DIEA, 1.75 ml, 10 mmol) and trimethylsilylethoxymethyl chloride (SEMCl, 1.83 ml, 10 mmol) are added, under argon, to a solution of 4-iodopyrazole (1.94 g, 10 mmol) in CH2Cl2 (100 ml). The mixture is stirred overnight at ambient temperature. The solvent is evaporated off under vacuum. The residue is taken up with a diethyl ether/water mixture. The organic phase, after drying and evaporation, gives a colourless oil which is purified by elution on silica gel with an EtOAc/CH2Cl2 (5/95) mixture. 3.02 g of product are obtained in the form of a colourless oil.

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, 4-Iodopyrazole, other downstream synthetic routes, hurry up and to see.

These common heterocyclic compound, 3469-69-0, name is 4-Iodopyrazole, 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. Computed Properties of C3H3IN2

Example 2: 4-((?)-2-(l-((2/?,3i?)-3-(2,4-Difluorophenyl)-3-hydroxy-4- (l/T-l,2,4-triazol-l-yl)butan-2-yl)-lflr-pyrazol-4-yl)vinyl)benzonitrileStep 1 : l-(l-Ethoxyethyl)-4-iodo-l//-pyrazole; 4-1OdO-IiZ-PyTaZoIe (3.Og) was suspended in benzene (15OmL) and the suspension was heated while stirring. Ethyl vinyl ether (4.4mL) was added thereto, concentrated HCl was added dropwise thereto, and the resulting mixture was stirred at 60 C for 3 hours. After completion of the reaction, the resulting mixture was concentrated by evaporation under a reduced pressure, and the residue was neutralized using aqueous saturated sodium hydrogen carbonate (1OmL). The resulting mixture was extracted with ethyl acetate (5OmL) and the extract was washed successively with distilled water (10OmL). The organic layer was dried over anhydrous magnesium sulfate and concentrated by evaporation under a reduced pressure. The resulting residue was purified by silica gel chromatography to obtain the title compound as a transparent yellow liquid (3.Og, yield 73%). 1H NMR (CDCl3): delta 7.54(s, IH), 7.41(s, IH), 5.40(q, IH, /=6.0 Hz), 3.38-3.18(m, 2H), 1.54(d, 3H, /=6.0 Hz), 1.05(t, 3H, /=7.1 Hz).

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

Application of 3469-69-0, 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. 3469-69-0, name is 4-Iodopyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a suspension of NaH (0.463 g, 15.47 mmol, 80% NaH/mineral oil) in DMF (100 mL) was added 4-iodo-pyrazole (1.0 g, 5.16 mmol) at 0 C under N2 atmosphere, the mixture was stirred at 0 C for 30 minutes, then iodomethane (0.64 mL, 10.31 mmol, d = 2.28) was added. The resulted mixture was warmed to rt and stirred overnight, then quenched with brine (100 mL), and concentrated in vacuo. The residue was diluted with EtOAc (200 mL) and washed with water (100 mL). The separated organic phase was concentrated in vacuo, and the residue was purified by a silica gel column chromatography (PE/EtOAc (v/v) = 2/1) to give the title compound as a light yellowish solid (490 mg, 45%). NMR (400 MHz, CDCb): delta 7.48 (s, 1H), 7.40 (s, 1H), 3.91 (s, 3H).

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

Electric Literature of 3469-69-0,Some common heterocyclic compound, 3469-69-0, name is 4-Iodopyrazole, molecular formula is C3H3IN2, 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.

1-(ethoxyethyl)-4-iodo-1H-pyrazole (20).; A 22 L 4-neck flask equipped with an mechanical stirrer, thermowell, N2 inlet and condenser was charged with 4-iodo-1H-pyrazole (14, 1.00 Kg, 5.16 mol) and toluene (10 L) and ethyl vinyl ether (18, 557 g, 740 mL, 7.73 mol, 1.5 equiv) was added. To the suspension 4 M HCl in dioxane (32 mL, 0.128 mol, 0.025 equiv) was added over 5 min with formation of a slightly thicker white suspension. The mixture was heated carefully to 35-40 C. at which point a mild exotherm to about 40 C. occurred with rapid dissolution of all solids to give a clear light yellow solution. The reaction mixture was heated at about 40 C. for an additional 0.5 hr until the GC analysis indicated the reaction was complete. The solution was allowed to cool to 25-30 C. and solid NaHCO3 (108 g, 1.29 mol, 0.25 equiv) was added. The suspension was stirred for 1 hr at room temperature to ensure the complete neutralization of HCl. The mixture was then filtered and the filtrate was concentrated under reduced pressure. The residual liquid was fractionally distilled to afford 1-(ethoxyethyl)-4-iodo-1H-pyrazole (20, 1.346 Kg, 1.373 Kg theoretical, 98%) as a pale yellow liquid (bp 89-93 at about 1 torr). For 20: 1H NMR (CDCl3, 250 MHz) delta ppm 7.61 (s, 1H), 7.47 (s, 1H), 5.46 (q, 1H, J=6.0 Hz), 3.48-3.23 (m, 2H), 1.60 (d, 3H, J=6.0 Hz), 1.11 (t, 3H, J=7.0 Hz); C7H11IN2O (MW, 266.08), LCMS (EI) m/e 267 (M++H).

The synthetic route of 3469-69-0 has been constantly updated, and we look forward to future research findings.

Related Products of 3469-69-0, 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. 3469-69-0 name is 4-Iodopyrazole, 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.

[00235] 4-lodopyrazole (10.0 g, 51 .55 mmol) was dissolved in 1 ,4-dioxane (40 mL) and to this was added potassium carbonate (7.12 g, 51 .55 mmol) followed by 4-methoxybenzyl chloride (6.99 mL, 51 .55 mmol) and the reaction was stirred at reflux overnight. Upon cooling, the reaction mixture was concentrated and the residue was partitioned between ethyl acetate and water. The organic phase was washed with brine, dried over sodium sulphate, filtered and evaporated to give a yellow oil. This was purified by column chromatography eluting with an ethyl acetate/hexane gradient, 0-30% ethyl acetate. Fractions containing product were combined and evaporated to give the title compound (9.20 g, 57%) as a straw coloured oil which crystallized on standing. 1 H NMR (400 MHz, DMSO-cf6) delta 7.98 (d, J= 0.7 Hz, 1 H), 7.52 (d, J= 0.7 Hz, 1 H), 7.28 – 7.17 (m, 2H), 6.98 – 6.85 (m, 2H), 5.24 (s, 2H), 3.73 (s, 3H).

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

Synthetic Route of 3469-69-0, 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. 3469-69-0, name is 4-Iodopyrazole belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

To a solution of 4-iodo-1H-pyrazole (7.00 g, 36.0 mmol) in 1,4-dioxane (30 mL) wasadded cyclopropylboronic acid (6.20 g, 72.0 mmol), cupric acetate monohydrate (9.40 g,47.0 mmol), 4-dimethylaminopyridine (108 mg, 43.0 mmol) and pyridine (3.50 g, 43.0 mmol) under nitrogen atmosphere. After stirred at 110 C overnight, the reaction mixture was cooled down to room temperature and diluted in water (50 mL), extracted with ethyl acetate (60 mL) for three times. The combined organic layers were washedwith brine (40 mL), dried over Na2 SO4() and filtered. The filtrate was concentrated under reduced pressure to give a crude product, which was purified by silica gel column chromatography (petroleum ether : ethyl acetate = 4 : 1) to afford the title compound (1.80 g, 21 % yield) as light yellow oil. ?HNMR (400 1VIHz, CDC13) 7.49 (s, 1H), 7.47 (s, 1H), 3.62- 3.57 (m, 1H), 1.13 – 1.08 (m, 2H), 1.05 – 0.99 (m, 2H).

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, 4-Iodopyrazole, other downstream synthetic routes, hurry up and to see.