Author: Jessica.F

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 49744-93-6 as follows. Product Details of 49744-93-6

Step 3 Ethyl 3-(4-cyanophenyl)-3-oxopropanoate (64 mg, 0.3 mmol) in THF (1 ml) and DMFDMA (0.3 mmol) was heated at 70 C. for 3 hours. The solution was added to a mixture of the guanidine from Step 2 (123 mg, 0.3 mmol), 1.0 M sodium ethoxide in ethanol (0.35 ml) and ethanol (1 ml). The mixture was then heated overnight at 80 C., cooled, diluted with dichloromethane, then washed with saturated sodium bicarbonate solution. The organic layer was concentrated in vacuo, redissolved in acetonitrile and the product precipitated with water. HPLC: 27.63 min (85% pure) MS: MH+=448 C22H21N7O4=447 g/mol

According to the analysis of related databases, 49744-93-6, 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. 459-22-3, name is 4-Fluorophenylacetonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 4-Fluorophenylacetonitrile

Reagents and conditions: (a) EtONa, EtOH, refluxing; (b) CH3NHNH2, HC1, EtOH,MW, 100C, 40 mm; (c) Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoyl chloride,DCM, then DBU. A mixture of 1.8 ml (15 mmol) of ethyl 2,2,2-trifluoroacetate (ib)and 0.96 g (7.1 mmol) of 2-(4-chloro-2-fluorophenyl)acetonitrile (3a) in 10 ml ofethanol was slowly dropped into hot solution of 1.2 g of sodium in 20 ml of ethanol.The mixture was refluxed overnight. The solution turns red. After cooled down, thesolution was poured into 250 ml of cold water acidified with 10 ml concentrated HC1.The mixture was extracted with ethyl acetate. The ethyl acetate extraction was washedwith water, brine and dried over Mg504. Ethyl acetate was removed and the residualreddish oil of 4,4,4-trifluoro-2-(4-fluorophenyl)-3 -oxobutanenitrile (3c) was obtained in1.3 g. The raw material was dissolved in 10 ml of ethanol and used in next step withoutfurther purification. A mixture of 2.8 ml of the above ethanol solution and 125pi ofmethylhydrazine with 0.2 ml of concentrated HC1 was irradiated in microwave oven at100C for 40 mm. The solution was treated with saturated NaHCO3 and extracted byethyl acetate. The organic layer was washed with water, brine, dried over Mg504 andconcentrated. The yellow residue was subjected to flash chromatography purificationwith MeOHIDCM to give 165 mg of 3-(trifluoromethyl)-4-(4-fluorophenyl)-1-methyl-1H-pyrazol-5-amine (3d) as light yellow solid. ?H NMR (500 MHz, CDC13) 7.32 (s,2H), 7.14 (t, J = 8.0 Hz, 2H), 3.76 (d, J = 33.5 Hz, 3H), 3.65 (s, 2H). M/Z =260.6(M+1). To a solution of Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoyl chloride (43mg, 0.20 mmol) produced from Fmoc-(R)-3-amino-4-(4-fluorophenyl)butanoic acid(from Chem Impex International) and thionyl chloride in 10 ml of anhydrous DCM were slowly added 3 -(trifluoromethyl)-4-(4-fluorophenyl)- 1-methyl-i H-pyrazol-5 – amine obtained as described above (39 mg, 0.15 mmol) in 5 ml of anhydrous DCM. The reaction mixture was stirred at room temperature overnight. The reaction mixture was quenched with methanol and solvents were removed. The residue was purified via silicagel with MeOHIDCM to obtained Fmoc protected product. Fmoc protected product was dissolved in 10 ml of ethyl acetate and 0.15 mmol of DBU was added. After 20mm 20 ml of ethyl acetate was added and mixture was washed with 20 ml of water. The organic layer was collected and solvent was removed. The residue was dissolved in MeOH and acidified with 0.2N HC1. The solution was purified via preparatory RP-HPLC, elutingwith H20/CH3CN gradient (+0.05% TFA). Product fractions are collected and concentrated. The residue is dissolved in a small amount of 2M HC1 in methanol and, after concentration in vacuo, 50 mg of Compound (3) is obtained as an HC1 salt. ?H NIVIR (500 IVIFIz, MeOD) 7.40 – 7.08 (m, 6H), 7.02 (t, J = 8.8 Hz, 2H), 3.77 (d, J = 15.4 Hz, 3H), 3.37 (dt, J = 7.9, 6.6 Hz, 1H), 2.64 (m, 2H), 2.42 (m, 2H). M/Z 439.4(M+i).

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.

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. 86770-80-1, name is 3,3-Difluorocyclobutanecarbonitrile, A new synthetic method of this compound is introduced below., Application In Synthesis of 3,3-Difluorocyclobutanecarbonitrile

Borane-THF (1 M in THF, 16.20 mmol, 16.20 mL) was added drop-wise over 5 minutes to a solution of 3,3- difluorocyclobutanecarbonitrile (14.70 mmol, 1.72 g) in (0889) THF (5 mL) under N2. The resulting solution was then heated to reflux for 20 hours then cooled in an ice-water bath. Methanol (20 mL) was added drop-wise. The (0890) resulting mixture was concentrated under reduced (0891) pressure. The residue was dissolved in methanol (10 mL) and concentrated hydrochloric acid (10 mL) and heated at reflux for 2 hours. The mixture was concentrated under reduced pressure and the residue azeotroped twice with ethanol before being suspended in diethyl ether. The resulting cream solid was isolated by filtration and dried under suction to give the title compound as a white solid (1.48 g, 64%)

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.

27387-23-1, name is 2-(2-Bromo-5-methoxyphenyl)acetonitrile, belongs to nitriles-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Quality Control of 2-(2-Bromo-5-methoxyphenyl)acetonitrile

To a solution of s2 in EtOH (10.0 mL) and H2O (5.0 mL) were successively added NaOH (2.94 g,73.5 mmol) and aqueous H2O2 (23 muL, 0.736 mmol) at room temperature. After the mixture washeated to reflux for 24 h, the reaction was quenched by addition of conc. HCl at 0 C. The crudemixture was extracted with EtOAc (x4) and the combined organic extracts were washed with brine,dried (Na2SO4), and concentrated in vacuo to give crude s3 (1.62 g) as pale yellow solid. Thiscrude material was used for next reaction without further purification.

The synthetic route of 27387-23-1 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. 2286-54-6, name is 3,3-Diphenylpropanenitrile, This compound has unique chemical properties. The synthetic route is as follows., Application In Synthesis of 3,3-Diphenylpropanenitrile

A solution of hydroxylamine hydrochloride (38.6 ml, 38.6 mmol) in MeOH was added to a solution of potassium hydroxide (38.6 ml, 38.6 mmol, Eq: 4) in MeOH at 0 C. The resulting mixture was filtered and the filtrate was added to a 150 mL round-bottomed flask containing 3,3-diphenylpropanenitrile (2 g, 9.65 mmol). The mixture was heated at reflux for 16 h, cooled and evaporated to dryness. The residue was dissolved in EtOAc, washed with brine, dried (MgSO4) and evaporated to dryness. The crude product was dissolved in CHCl3 (50 ml), treated with dimethyl but-2-ynedioate (1.65 g, 11.6 mmol, Eq: 1.2) and heated at reflux for 1 h and then evaporated to dryness. The residue was dissolved in xylene (10 ml), heated at 120 C. in a microwave oven for 4 h and evaporated to dryness. Chromatography (80 g SiO2; 20 to 100% EtOAc in hexanes) gave the title product as an off-white solid (0.42; 12%). LCMS: m/z=348.9 (MH+).

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 2286-54-6.

Adding a certain compound to certain chemical reactions, such as: 77429-04-0, name is Ethyl 3-chloro-2-cyano-4,4,4-trifluorobut-2-enoate, 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 77429-04-0, HPLC of Formula: C7H5ClF3NO2

To a mixture of 21 g of ethyl 3-chloro-2-cyano-4,4,4-trifluorobut-2-enoate and 7.6 g of 4- nitrobenzimidamide in 300 ml of water, 31 ml of a aqueous sodium hydroxide solution (2M) were added. The reaction mixture was stirred at RT for 4 h, then diluted with 200 ml of water, acidified with half-concentrated aqueous hydrochloric acid to pH 3 and extracted with EtOAc (3 x 500 ml). The combined organic layers were dried over magnesium sulfate and the solvents were removed under reduced pressure. The crude product was purified by chromatography on silica gel eluting with a gradient of EtOAc/methanol. Yield: 2.7 g.

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.

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. 508203-48-3, name is 2,3-Difluoro-4-methylbenzonitrile, A new synthetic method of this compound is introduced below., Product Details of 508203-48-3

To a suspension of 2,3-difluoro-4-methylbenzonitrile (5.0 g, 32.6 mmol) in ethanol (111 mL) at 25C was added hydroxylamine hydrochloride (4.5 g, 65.3 mmol). The reaction mixture was heated at80C for 2 h. After cooling to room temperature the volatiles were removed under reduced pressurethus affording a white solid that was used in the next step without purification.1H NMR (400 MHz, CDCI3) oe ppm: 7.30 (m, 1H), 6.95 (m, 1H), 6.50 (brs, 1H), 5.05 (brs, 2H),2.30 (s, 3H).

The synthetic route of 508203-48-3 has been constantly updated, and we look forward to future research findings.

Application of 159847-80-0, 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. 159847-80-0, name is Methyl 4-amino-3-cyanobenzoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

4-Amino-3-cyano-benzoic acid methyl ester (3.2 g, 10 mmol) in tetrahydrofurane/ water (110 ml, 1:1) was added lithium hydroxide hydrate (2.3 g, 30 mmol), the reaction mixture was stirred at room temperature for 20 hours and added hydro chloric acid (1 M) to pH = 3. From the mixture was tetrahydrofurane distilled of and the title compound precipitated out of solution.

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, Methyl 4-amino-3-cyanobenzoate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 220239-65-6,Some common heterocyclic compound, 220239-65-6, name is 4-fluoro-3-(trifluoromethyl)phenylacetonitrile, molecular formula is C9H5F4N, 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.

EXAMPLE H1 Preparation of 2-(4-fluoro-3-trifluoromethyl-phenyl)-ethylamine hydrochloride A solution of (4-fluoro-3-trifluoromethyl-phenyl)-acetonitrile (4.00 g, 19.3 mmol) in THF was added dropwise at 0-5 C. to a suspension of lithium aluminum hydride (1.61 g, 42.4 mmol) in diethyl ether (20 mL). The ice bath was removed and the reaction mixture was allowed to reach RT, then heated at reflux overnight. After cooling to 0 C., saturated aq. sodium sulfate solution was carefully added. After the initial exothermic reaction had subsided, the flask was allowed to warm to ambient temperature and solid magnesium sulfate (dry) was added to dry the suspension, which was subsequently filtered and washed with diethyl ether. After removal of the solvent, the residue was dissolved in diethyl ether (50 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 8 mL), and evaporated to dryness, leading to a solid orange foam. This residue was dissolved in dichloromethane (200 mL), and treated with water (100 mL), followed by 1 M aq. hydrochloric acid solution (50 mL), and stirred for 15 minutes, then the organic layer was separated and extracted a second time with 1 M aq. hydrochloric acid solution (50 mL). The combined aqueous phases were then washed with dichloromethane (50 mL), treated with concentrated aq. sodium hydroxide solution to adjust the pH to 12, and extracted twice with dichloromethane. The combined organic phases were washed with water and dried over magnesium sulfate. After filtration and evaporation of the solvent, the residue was dissolved in diethyl ether (5 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether, 2 mL), and stirred for 10 min. The precipitate was collected by filtration and dried to afford the title compound (632 mg, 13%). White solid, MS (ISP) 208.2 (M-Cl)+.

The synthetic route of 220239-65-6 has been constantly updated, and we look forward to future research findings.

Application of 1105665-42-6, These common heterocyclic compound, 1105665-42-6, name is 5-Bromo-2,3-difluorobenzonitrile, 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.

2,3-difluoro-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile (0275) To a solution of 5-bromo-2,3-difluorobenzonitrile (140 mg, 0.64 mmol) in 1,4-dioxane (7 mL) were added 4,4,5,5-tetramethyl-2-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1,3,2-dioxaborolane (179.4 mg, 0.71 mmol), Pd(dppf)Cl2 (26.2 mg, 0.04 mmol) and potassium acetate (126 mg, 1.28 mmol) at room temperature. The resulting mixture was stirred for 2 h at 120 C. and then water (10 mL) was added. The mixture was extracted with ethyl acetate (30 mL×3). The organic phases were combined, washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure to yield 2,3-difluoro-5-(tetramethyl-1,3,2-dioxaborolan-2-yl)benzonitrile as brown oil (200 mg, crude). MS: m/z=266.0 [M+H]+.

The synthetic route of 1105665-42-6 has been constantly updated, and we look forward to future research findings.