Month: April 2021

Application of 17417-09-3, A common heterocyclic compound, 17417-09-3, name is 2-Fluoro-5-nitrobenzonitrile, molecular formula is C7H3FN2O2, 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.

To a solution of 2(H)-1,2,3-triazole (0.913 g, 13.24 mmol) in DMF (15 mL) was added portionwise sodium hydride (60% suspension in mineral oil, 0.530 g, 13.24 mmol) at rt and then stirred the mixture for 1H at room temperature. The reaction mixture was then cooled back down to OeC, and a solution of 2-fluoro-5-nitrobenzonitrile (2.0 g, 12.04 mmol) in DMF (10 mL) was added dropwise. The resulting mixture was stirred for 1.5 h at OeC and then at RT for 1.5 h. The mixture was quenched with ice cooled water and extracted with EtOAc (2/150 mL). The combined organic layers were washed with water (2/1,50 mL), brine (50 mL), dried (Na2SC>4) and filtered. The filtrate was rotary evaporated to leave a crude which was purified by flash column chromatography (silica gel, 20-30% EtOAc in hexanes as eluent) to give 5-nitro-2-(2H-1,2,3-triazol-2-yl)benzonitrile (1.2 g, 46.3% yield) & 5-nitro-2-(1H-1,2,3-triazol-1-yl)benzonitrile (0.7 g, 27.0% yield). 5-nitro-2-(2H-1,2,3-triazol-2-yl)benzonitrile: 1HNMR (400 MHz, DMSO-d6) ||8.93 (d, J = 2.5 Hz, 1H), 8.68 (dd, J = 8.5, 2.5 Hz, 1H), 8.44 (s, 2H), 8.40 (d, J = 8.5 Hz, 1H). ESI-MS (m/z) 216.04 (MH)+. 5-nitro-2-(1H-1,2,3-triazol-1-yl)benzonitrile: 1HNMR (400 MHz, DMSO-d6) ||9.05 (d, J = 2.5 Hz, 1H), 8.95 (d, J = 1.3 Hz, 1H), 8.75 (dd, J = 8.5, 2.5 Hz, 1H), 8.20 (d,J = 8.5 Hz, 1H), 8.15 (d, J = 1.3 Hz, 1H); ESI-MS (m/ z) 216.00 (MH)+.

The synthetic route of 17417-09-3 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. 1558-82-3, name is Ethyl N-cyanoacetimidate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: Ethyl N-cyanoacetimidate

A mixture of 1.2 g (0.004 mol) of 2-chloro-4,5,6,7-tetrahydrothiazole [5,4-c] pyridine trifluoroacetate,0.67 g (0.006 mol)N-cyanoethyl esterWas added to a reaction flask equipped with 30 ml of methanol,0.73 g (0.0048 mol) of DBU was added,Heating to reflux reaction,After 2 hours the TLC monitoring reaction was complete,Cooling white solid precipitation, the filter that white solid 0.49g,

According to the analysis of related databases, 1558-82-3, the application of this compound in the production field has become more and more popular.

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. 6393-40-4, name is 4-Amino-3-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Formula: C7H5N3O2

A mixture of 4-amino-3-nitrobenzonitrile (63.3 g, 388 mmol) in 1,4-dioxane (600 mL) and anhydrous ethanol (600 mL) was cooled in an ice water bath to 0-5 C and treated with gaseous HCl for 1.5 h. The reaction mixture was tightly sealed and allowed to warm up to room temperature with stirring for 18 h. The flask was then carefully unsealed and the reaction mixture was diluted with anhydrous diethyl ether (about 2.4 L) until a cloudy solution was obtained. A minimum amount of absolute ethanol required to give a clear solution was then added, and the resulting solution stirred until crystals of 4-amino-3-nitro- benzimidic acid ethyl ester were observed. Ether was then cautiously added to complete the crystallization process and the suspension was allowed to stand for about 30 minutes. The crystals were filtered and washed with dry diethyl ether, then allowed to dry under aspirator vacuum. The crystals were dried in vacuo to give 4-amino-3-nitro-benzimidic acid ethyl ester hydrochloride (84.6 g) as off-white crystals.

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.

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. 939-80-0, name is 4-Chloro-3-nitrobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 939-80-0

[00200] 4-(2,5-Difluorophenoxy)-3-nitrobenzonitrile 21. A solution of 4-chloro-3- nitrobenzonitrile (5 g) in THF (200 mL) at room temperature was treated with K2CO3 (19 g), followed by 2,5-difluorophenol (3.7 g). After stirring at room temperature for 18 hrs, the solid was filtered off and rinsed with copious amounts of EtOAc. The filtrate was washed sequentially with saturated aqueous NaHCU3 solution, water, and saturated aqueous NaCl solution, dried over anhydrous Na2SO4, filtered, and concentrated in vacuo. The residual was triturated with hexanes and collected by suction to furnish the desired product 21, which was used directly in the next step without further purification.

The synthetic route of 939-80-0 has been constantly updated, and we look forward to future research findings.

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. 85068-32-2, name is 2-(3,5-Bis(trifluoromethyl)phenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: nitriles-buliding-blocks

[0094] 0.50 g (1.57 mmol) of Nile Red, 0.40 g (1.57 mmol) of 3,5-bis(trifluoromethyl)phenylacetonitrile, and 25 ml of acetic anhydride were placed in a 100 ml pear-shaped flask. The solution in the pear-shaped flask was heated in a silicone oil bath to 135 C. and allowed to react for 4 hours. Acetic an hydride was distilled away with an evaporator and the remaining was dissolved in chloroform. This chloroform solution was washed with a 5% aqueous solution of sodium hydroxide and then with water. After the addition of sodium sulfate, the solution was allowed to stand for 30 minutes to be dried. The dried solution was concentrated with an evaporator. The obtained solid was purified by a column chromatography that used silica gel and benzene. 30 mg of violaceous solid was obtained in a 12% yield. The melting point of the product was 257-260 C. A 1H-NMR spectrum and an IR spectrum of this product are shown in FIGS. 1 and 2. The results of elemental analysis of this product are as follows. Based on these results, the obtained product was identified as the chemical compound represented by formula (12). [0095] The results of elemental analysis [0096] Found values: C: 66.03, H: 4.31, N: 5.16 [0097] Calculated values: C: 65.91, H: 4.20, N: 5.30

The synthetic route of 85068-32-2 has been constantly updated, and we look forward to future research findings.

Application of 6629-04-5, 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. 6629-04-5 name is N-Cyanoacetylurethane, 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.

Compound 18 (0.5 g, 1.58 mmol) and concentrated hydrochloric acid (7 ml) were added to water (15 ml), and the solution was dropped to 0.After C, an aqueous solution of sodium nitrite (0.143 g, 2.05 mmol, 2 ml) was slowly added dropwise to the above solution, and the reaction was carried out for 0.5 h.In a reactor, compound 10 (0.246 g, 1.58 mmol), pyridine (5 ml), water (15 ml) was added thereto, and the solution was lowered.To 0 C, then the reaction solution in the previous reactor was quickly poured into it, and the reaction was stirred for 0.5 h. After the reaction was completed, ethyl acetate(30 ml × 2) was extracted, and the organic phases were combined, dried, and dried to give an orange-yellow solid, 0.48 g, yield 63%.

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

Electric Literature of 38487-86-4, 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. 38487-86-4, name is 2-Amino-4-chlorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: 2-Aminobezonitrile derivatives (1 mmol),substituted carbonyl compounds (1.5 mmol) and [Nbmd][OH] (1 mL) werestirred at room temperature. The progress of the reaction was monitored byTLC under UV light. After completion of the reaction the mixture was extractedwith ethyl acetate (3 x 10 mL) and washed with water (3 x 10 mL). Thecombined extract was dried over anhydrous Na2SO4. The filtrate wasconcentrated under reduced pressure. The product was purified by columnchromatography over silica gel using n-hexane/ethyl acetate (3:1 v/v) aseluent to get the purified product. The products were then characterized byESI-MS, 1H NMR, 13C NMR and 1F NMR spectra.

The synthetic route of 2-Amino-4-chlorobenzonitrile has been constantly updated, and we look forward to future research findings.

Reference of 668-45-1, The chemical industry reduces the impact on the environment during synthesis 668-45-1, name is 2-Chloro-6-fluorobenzonitrile, I believe this compound will play a more active role in future production and life.

To a solution of A5.1 (1.55 g, 10.0 mmol) in 100 mL of anhydrous methanol was added sodium methoxide (4.32 g, 80 mmol). The mixture was heated at 85 oC and stirred overnight, then concentrated under reduced pressure to remove solvents. The residue was diluted with 400 mL DCM, washed with Sat. NH4Cl (2 × 20 mL), dried over anhydrous Na2SO4, concentrated under vacuum. The crude product was purified by column chromatography (PE:EA =10:1) to give the title compound (1.5 g, 89.8%) as a pale yellow solid. LC-MS: [MH]+ = 168.0

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, 2-Chloro-6-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Related Products of 630-18-2, A common heterocyclic compound, 630-18-2, name is Pivalonitrile, molecular formula is C5H9N, 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 4-bromobiphenyl 1a (3.0 mmol, 699.3 mg) in THF (3.0 mL) was added n-BuLi (4.5 mmol, 1.55 M in hexane, 2.87 mL) at 50 C. The obtained mixture was stirred for 30 min at 50 C under an argon atmosphere. Pivalonitrile (6.0 mmol, 498.8 mg) in THF (2.0 mL) was added to the mixture at 50 C and the obtained mixture was stirred for 30 min in the temperature range of 50 C to room temperature. MeOH (2.0 mL) was added to the mixture. Then, I2 (12.0 mmol, 3045.6 mg) and K2CO3 (12.0 mmol, 1658.4 mg) were added to the mixture at room temperature, and the obtained mixture was stirred for 6 h at 70 C. Sat. aq. Na2SO3 solution (20.0 mL) was added to the reaction mixture, and the product was extracted with AcOEt (10.0 mL x 3). The organic layer was dried over Na2SO4. After filtration and removal of the solvent, the residue was purified by silica-gel column chromatography (chloroform: n-hexane 1:1) to give 4-cyanobiphenyl 2a (451.6 mg, 84%).

The synthetic route of 630-18-2 has been constantly updated, and we look forward to future research findings.

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. 78881-21-7, name is 4-Amino-3-methylbenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H8N2

A solution of sodium nitrite (0.52 g, 7.57 mmol) in water (3 ml.) was added dropwise to a cold (0C) mixture of 4-amino-3-methylbenzonitrile (1 g, 7.57 mmol) and concentrated HCI (12 ml.) keeping the internal temperature below 0C. After 5 min stirring, tin dichloride dihydrate (3.75 g, 16.6 mmol) in concentrated HCI (4 ml.) was added at 0C. The reaction mixture was allowed to warm to rt and stirred for 2 h. The resulting precipitate was collected by vacuum filtration and dried to provide 500 mg of the title compound. tR: 0.24 min (LC-MS 2); ESI-MS: 148 [M+H]+(LC-MS 2).

The synthetic route of 78881-21-7 has been constantly updated, and we look forward to future research findings.