Author: Jessica.F

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.

Electric Literature of 1009-35-4, 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. 1009-35-4, name is 4-Fluoro-3-nitrobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

A mixture of 4-fluoro-3-nitrobenzonitrile (5.0 g, 30.1 mmol) and Fe powder (5.05 g, 90.3 mmol) in AcOH (100 mL) was heated at 80 C. for 1 hour under N2. Then the solvent was removed under vacuum and water (200 mL) was added to the residue. The solution was adjusted to pH 6 by addition of Na2CO3 and extracted with DCM (2×200 mL). The organic layers were combined, dried over Na2SO4, filtered and concentrated to yield 3-amino-4-fluorobenzonitrile (48), which was used without further purification. MS m/z 137.0 (M+1)+.; To a stirring suspension of imidazo[1,2-a]pyridine-3-carboxylic acid (1) (3.0 g, 18.5 mmol) in anhydrous dichloromethane (50 mL) at 0 C. was added dropwise oxalyl chloride (4.84 mL, 55.5 mmol). Then, three drops of anhydrous DMF was added and the reaction mixture was stirred at room temperature for 15 minutes. The solvent was concentrated and the crude solid was added to a stirring solution of 3-amino-4-fluorobenzonitrile (48) (2.5 g, 18.5 mmol) in anhydrous pyridine (50 mL) at room temperature. The reaction was stirred for 20 minutes and quenched with water (200 mL) with stirring for another 10 minutes. Then the precipitate was filtered and dried in air to yield N-(5-cyano-2-fluorophenyl)imidazo[1,2-a]pyridine-3-carboxamide (49). 1H NMR (400 MHz, d6-DMSO) delta 10.40 (s, 1H), 9.43 (td, J=1.2, 6.8 Hz, 1H), 8.63 (s, 1H), 8.21 (dd, J=2.0, 7.2 Hz, 1H), 7.78-7.84 (m, 2H), 7.54-7.63 (m, 2H), 7.22 (dt, J=1.2, 6.8, 1H). MS m/z 281.1 (M+1)+.; NH2OH (10 mL, 32.1 mmol) was added in one portion to a stirred suspension of N-(5-cyano-2-fluorophenyl)imidazo[1,2-a]pyridine-3-carboxamide (49) (3.6 g, 12.85 mmol) in EtOH (100 mL). The resulting suspension was heated at 70 C. for 3 hours and then the solvent was removed to yield N-(2-fluoro-5-(N?-hydroxycarbamimidoyl)phenyl)imidazo[1,2-a]pyridine-3-carboxamide (50). 1H NMR (400 MHz, d6-DMSO) delta 10.21 (s, 1H), 9.70 (s, 1H), 9.45 (td, J=1.2, 7.2 Hz, 1H), 8.61 (s, 1H), 7.95 (dd, J=2.4, 7.6 Hz, 1H), 7.79 (td, J=1.2, 8.8 Hz, 1H), 7.51-7.60 (m, 2H), 7.31-7.37 (m, 1H), 7.19 (dt, J=1.2, 6.8, 1H), 5.88 (s, 2H). MS m/z 314.1 (M+1)+.

The chemical industry reduces the impact on the environment during synthesis 4-Fluoro-3-nitrobenzonitrile. I believe this compound will play a more active role in future production and life.

Application of 6393-40-4, These common heterocyclic compound, 6393-40-4, name is 4-Amino-3-nitrobenzonitrile, 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.

In DMF (20 ml), 3-nitro-4-aminobenzonitrile (1.12 g) was dissolved, and the solution was added with 60% sodium hydride (411 mg), followed by stirring at room temperature for 30 minutes. The solution was added with 1-iodopropane (805 mul) and stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was then dissolved in ethyl acetate. The resultant was washed with water and then subjected to extraction with ethyl acetate. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure, thereby obtaining a crude product (1.58 g) of the subject compound as a yellow solid. MS(FAB,Pos.):m/z=206[M+H]+

Statistics shows that 4-Amino-3-nitrobenzonitrile is playing an increasingly important role. we look forward to future research findings about 6393-40-4.

Some common heterocyclic compound, 57381-37-0, name is 2-Bromo-5-chlorobenzonitrile, molecular formula is C7H3BrClN, 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. Quality Control of 2-Bromo-5-chlorobenzonitrile

GammaAlpha1 l-(2-Bromo-5-chloro-phenyl)- 1-methyl-ethylamine To a stirred solution of 2-bromo-5-chloro-benzonitrile (10 g, 46 mmol) in THF (200 mL) at 0 C, was added MeMgBr (77 mL, 230 mmol) drop wise. The reaction mixture was allowed to warm up to room temperature and stirred for 2 hours. Ti(Oi-Pr)4 (13 g, 46 mmol) was added and the solution was stirred for another 16 hours before it was quenched with aq. HC1 solution and washed with EtOAc. The aqueous phase was adjusted to pH ~ 10 with aq. NaOH solution, and exacted with EtOAc (3x). The combined organic layers were concentrated to give a crude title product (3.8 g, 33%) as oil, which was used directly in the next step without further purification. MS: 249.30 (M+H)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 57381-37-0, its application will become more common.

Application of 16532-79-9, 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. 16532-79-9 name is 4-Bromophenylacetonitrile, 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.

EXAMPLE 8 Synthesis of N2- ( (1S)-L- {4 – [L- (AMINOCARBONYL) CYCLOPROPYL] BIPHENYL-4-YL}-2, 2, 2-TRIFLUOROETHYL)-NL-(L- cyanocyclopropyl) -4-fluoro-L-leucinamide Step 1 : Preparation of 1-(4-bromophenyl)cyclopropanecarbonitrile; To a room temperature solution of 4-bromophenylacetonitrile (18.0 g) in 22 ML of sodium hydroxide (50% in water W/W) were added 1-BROMO-2-CHLOROETHANE and (12.0 mL) and benzyltrimethylammonium chloride (627 mg). The mixture was heated at 60 C overnight. The reaction mixture was cooled to room temperature and diethyl ether was added (300 mL. The ether layer was washed with water (100 ML), hydrogen chloride (100 ML, 10% HC1 in water) and brine. The organic layer was dried with magnesium sulfate and the solvent removed in vacuo. The residue was purified by trituration using diethyl ether and hexanes to yield the title compound. H NMR (CD3COCD3) 8 7.60 (2H, d), 7.35 (2H, d), 1.74-1. 80 (2H, m), 1.52-1. 57 (2H, m).

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