Category: nitriles-buliding-blocks

Adding a certain compound to certain chemical reactions, such as: 116332-64-0, name is 4-Cyano-N-methoxy-N-methylbenzamide, belongs to nitriles-buliding-blocks 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 116332-64-0, Quality Control of 4-Cyano-N-methoxy-N-methylbenzamide

To a -780C stirred solution of trimethyl (2-methylbut-3-yn-2-yloxy) silane (3.3 g, 20.00 mmol) in dry THF (45 mL), «-BuLi (4.1 mL, 9.00 mmol, 1.6 M in hexane) was added dropwise over 10 minutes under an inert atmosphere. The reaction mixture was stirred for 30 min at -78 0C, and then a solution of 4-cyano-N-methoxy-N-methylbenzamide (2.0 g, 10.00 mmol) in dry THF (15 mL) was added to the reaction mixture and stirring was continued for an additional 1 h at -78 0C. The reaction mixture was quenched with a saturated NH4Cl solution and extracted with EtOAc (2 x 100 mL). The combined organic layers were washed with water (50 mL) and brine (50 mL), dried OVCr Na2SO4, filtered, and concentrated in vacuo to obtain the crude product. The crude material was purified via silica gel column chromatography eluting with 15 % EtOAc in hexanes to afford 4-(4- methyl-4-(trimethylsilyloxy) pent-2-ynoyl) benzonitrile (3.8 g, 68 %) as a yellow oil.

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

Application of 33279-01-5,Some common heterocyclic compound, 33279-01-5, name is 3-Oxopentanenitrile, molecular formula is C5H7NO, 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 3-oxopentanenitrile (0.74 g, 7.6 mmol) and quinolin-5-yl-hydrazine (prepared from Example 4 step a, 1.0 g, 6.3 mmol) in ethanol (5 mL) was heated at 80 C. for 3 h with stirring. After cooling to room temperature, 20% aqueous sodium hydroxide (1.5 mL) was added to the reaction mixture and then heated at 70 C. for 3 h. The reaction mixture was cooled to room temperature and concentrated in vacuo. The crude residue was dissolved in 1:1 dichloromethane/methanol (40 mL) and the phases were separated. The organic layer was dried (Na2SO4), and filtered through a pad of Celite. The filtrate was concentrated in vacuo and the crude residue was purified by flash chromatography (SiO2, 1-10% methanol containing 10% ammonium hydroxide in dichloromethane) to give the desired product (0.83 g, 3.5 mmol, 55%).

The synthetic route of 33279-01-5 has been constantly updated, and we look forward to future research findings.

Reference of 3759-28-2,Some common heterocyclic compound, 3759-28-2, name is 2-(Cyanomethyl)benzonitrile, molecular formula is C9H6N2, 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 homophthalonitrile 2 (129 mg, 0.82 mmol) in PriOH (4 ml), salicylaldehyde 1 (2.46 mmol) and NH4OAc (143 mg, 1.64 mmol) were added. The mixture was placed into a microwave reactor and heated at 150 C for 10 min. The vessel was opened, MeNO2 (0.439 ml, 8.2 mmol) and Et3N (0.114 ml, 0.82 mmol) were added, the mixture was heated again in the microwave reactor at 150 C for 10 min. The solvent was evaporated under reduced pressure, the residue was chromatographed on silica gel (EtOAc-hexane, 1:5-1:1) (method A) or was dissolved in asmall volume of Et2O or CH2Cl2 and extracted with HCl aqueous solution(0.6 m, 3 30 ml). The aqueous layer was neutralized with Na2CO3. The precipitate was filtered off and washed with H2O several times and once with a small amount (1.5 ml) of PriOH and dried in air (method B).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2-(Cyanomethyl)benzonitrile, its application will become more common.

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 4553-07-5 as follows. Formula: C11H11NO2

A slurry of sodium hydride (60% dispersion in mineral oil, 811 mg, 20.2 mmol) in dry THF (170 mL) at 0C was added with ethyl 2-cyano-2-phenylacetate (3.2 g, 16.9 mmol). The resulting mixture was stirred for one hour at 0C before adding methyl iodide (2.87 mL, 30.3 mmol) dropwise and slowly warming the mixture to roomtemperature over 16 hours. The mixture was then quenched with saturated aqueous NH4C1 (100 mL) and EtOAc (200 mL). The layers were separated and the aqueous phase was back-extracted with EtOAc (3 x 50 mL). The combined organic phases were dried (MgSO4), filtered and the solvent was removed in vacuo. The residue was purified by silica gel colunm chromatography, eluting with 10% EtOAc in isohexane to give the titlecompound as a colourless oil (2.2 g, 64%).?H NMR (400 MHz, CDC13): oe 7.55-7.5 1 (m, 2 H), 7.44-7.36 (m, 3 H), 4.26-4.22 (m, 2 H), 1.96 (s, 3 H), 1.25 (t, J = 7.2 Hz, 3 H).

According to the analysis of related databases, 4553-07-5, the application of this compound in the production field has become more and more popular.

Application of 185836-35-5, A common heterocyclic compound, 185836-35-5, name is 4-(Benzyloxy)-2-fluorobenzonitrile, molecular formula is C14H10FNO, 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.

5.1. 2-[[(1-Methylethylidene)amino]oxy]-4-(phenylmethoxy)benzonitrile A solution of 7.83 g (0.107 mol) of acetone oxime in 200 ml of dimethylformamide is stirred for 30 minutes in the presence of 12 g (0.11 mol) of 95% potassium t-butanolate. A solution of 20.3 g (0.089 mol) of 2-fluoro-4-(phenylmethoxy)benzonitrile in 100 ml of dimethylformamide is then added over 15 minutes. The mixture is stirred for 2 hours and then poured into ice-water. The crystalline product is filtered off and dissolved in dichloromethane, and the solution is then dried over sodium sulphate and concentrated under reduced pressure. 21.2 g of product are obtained. Melting point: 102 C.

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.

These common heterocyclic compound, 105942-08-3, name is 4-Bromo-2-fluorobenzonitrile, 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 C7H3BrFN

a) 4-Bromo-2-methoxybenzonitrile A suspension of potassium methoxide (4.24 g, 60.0 mmol) in tetrahydrofuran (40 mL) was added in portions to a solution of 4-Bromo-2-fluorobenzonitrile (8.0 g, 40.0 mmol) in tetrahydrofuran (50 mL) at -50° C. After one hour, the dry ice bath was removed and the reaction mixture was allowed to warm up to room temperature and stirred at room temperature for 6 hours. The reaction mixture was poured onto water (250 mL) and the solid was collected by filtration to give 4-bromo-2-methoxybenzonitrile (7.85 g, 92percent). 1H NMR (DMSO-d6) delta 3.94(s, 3H), 7.32 (d, J=8.23 Hz, 1H), 7.15 (s, 1H), 7.69 (d, J=8.23 Hz, 1H).

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

Reference of 64113-84-4, 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. 64113-84-4, name is 2-Fluoro-5-methylbenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 27 N-(2-Cyano-4-methylphenyl)-4-piperidone propylene ketal (29) A solution of 2-fluoro-5-methylbenzonitrile (2.76 g, 20.4 mmol) and 4-piperidone propylene ketal (3.39 g, 21.5 mmol) in DMF (50 mL) was heated in an oil bath (90 C., 20 h). The mixture was diluted with ether and sodium carbonate solution. The aqueous layer was extracted with two additional portions of ether and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. PCTLC (SiO2, 6 mm, 50-0% hexane/CHCl3) afforded the title compound (29). 1H NMR (CDCl3, 400 MHz) consistent with assigned structure. FABLRMS m/e 273 g/mole (M++H, C16H20N2O2=273 g/mole.) HPLC (Vydac; C18; diameter=4.6 mm; length=150 mm; gradient=H2O [0.1% H3PO4]-CH3CN, 95%-5%, 5%-95%, over 16 minutes, 2 ml/min flow rate) RT=9.97 min; focus=215 nm; 97.8% pure.

The chemical industry reduces the impact on the environment during synthesis 2-Fluoro-5-methylbenzonitrile. I believe this compound will play a more active role in future production and life.

Related Products of 159847-81-1,Some common heterocyclic compound, 159847-81-1, name is Methyl 2-amino-5-cyanobenzoate, molecular formula is C9H8N2O2, 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 methyl 2-amino-5-cyanobenzoate (5.68 mmol) in DCM (lOmL) was added triethyamine (8.52 mmol) followed by methyl 3-chloro-3-oxopropionate (7.38 mmol). The resulting reaction mixture was stirred at ambient temperature overnight. The reaction mixture was partitioned between EtOAc and IM HCI and the layers then separated. The organic layer washed sequentially with saturated aqueous NaHCO, followed by brine. The organic layer was diied over Na2S04, filtered, and concentrated in vacuo. The resulting residue was carried on without further purification. [00170] The residue from above was treated with 0.5M NaOMe in MeOH (6.83 mmol). The heterogenous mixture was stirred at ambient temperature for 30 min. Diethyl ether was then added to the reaction mixture and the solid was collected via vacuum filtration, washing with ether. The obtained solid was carried on without further purification. [00171] To a flask containing the solid from above cooled to 0 C was added POCK (15 mL). The mixture became warm and bubbled. The resulting reaction mixture was heated to 90C for 3 h. Cooled the dark reaction mixture to ambient temperature and poured it very slowly into stirring saturated aqueous NaHCOj cooled to 0 C. Solid NaHCQs was then added until the solution was basic. The aqueous solution was extracted with EtOAc (3x). The combined organic layers were dried over a2S04, filtered, and concentrated in vacuo. The obtained residue was purified via flash column chromatography, eluting with 9: l/hexanes:EtOAc, to yield the intermediate 13 (29% over 3 steps). MS ESI (m/z) 281 (M+ J ); ;H NMR (300 MHz, CDCi3) 5 8.63 (d, 1 H, J=l .8 Hz), 8.16 (d, 1H, ./ 8 · Hz), 8.00 (dd, lH, Hz), 4.08 (s, 3H); i C NMR (CDC , 75MHz) 5 163.4, 148.9, 148.1 , 141 .8, 1 33.3, 130.8, 130.6, 128.8, 124.3, 1 17.7, 1 12.8, 54.1.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-amino-5-cyanobenzoate, its application will become more common.

Synthetic Route of 4640-66-8, 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. 4640-66-8, name is 4-Chlorophenacylcyanide, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a mixture of appropriate beta-ketonitrile (6a-c, 5.5mmol) and substituted hydrazine or hydrazine hydrochloride(6 mmol) in 20 mL of ethanol was added aqueous 2 M HCl(0.8 mL). The resulting solution was heated at 100 C for 4h. After cooling to room temperature, the mixture was concentrated under reduced pressure. The residue was poured into ice water and basified with aqueous 10% NaOH. The resulting suspension was extracted with diethyl acetate (3 x20 mL). The combined organic layers were dried over Na2SO4 and then concentrated under reduced pressure to afford the title aminopyrazoles, which were purified by crystallization from ethanol.

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

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. 6393-40-4, name is 4-Amino-3-nitrobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., category: nitriles-buliding-blocks

A solution of 4-amino-3-nitrobenzonitrile (1) (3.0 g) in ethanol (80 mL) was sparged for 5 minutes with nitrogen. Palladium on carbon (10%, 300 mg) was added and the mixture was saturated with hydrogen. The mixture was stirred under a hydrogen balloon for seven hours. The mixture was sparged with nitrogen and filtered through celite. The filtrate was concentrated in vacuo to provide the title compound, 3,4- diaminobenzonitrile (2).

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 6393-40-4.