Month: May 2021

Reference of 32446-66-5, 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. 32446-66-5, name is 4,4′-Dicyanobenzophenone, This compound has unique chemical properties. The synthetic route is as follows.

EXAMPLE 3 4-[alpha-(4-Cyanophenyl)-alpha-hydroxy-5-thiazolylmethyl]-benzonitrile Analogously to Example 1, the title compound is prepared starting from 0.512 ml of diisopropylamine, 2.44 ml of a 1.6M n-butyllithium solution, 530 mg of 2trimethylsilylthiazole and 603 mg of 4,4′-dicyanobenzophenone in THF at -70 and with working up in the same manner. Purification of column chromatography (SiO2, hexane/ethyl acetate 2:2) yields the title compound in pure for. TLC (hexane/ethyl acetate 2:2) Rf =0.2; 1 H-NMR (CDCl3): delta(ppm)=4.39 (s,1H), 7.42 (d,1H), 7.54 and 7.7 (m,8H), 7.88 (d,1H).

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

Synthetic Route of 133541-45-4, A common heterocyclic compound, 133541-45-4, name is 4-Bromo-2,5-difluorobenzonitrile, molecular formula is C7H2BrF2N, 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 suspension of sodium hydride (4.04 g, 100 mmol, 60 % purity) in THF (25 mL) was added tert-butyl N-(2-hydroxypropyl)carbamate (8.84 g, 50.5 mmol) at 0 “C. The resulting mixture was stirred at 0 C for 0.5 h, then a solution of 4-bro mo-2,5-difluorobenzonitrile (10 g, 45.9 mmol) in THF (25 mL) was added. The mixture was stirred at 0 C for 0.5 h. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to give a residue, which was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 50/1 to 10/1 ) to give the desired product (13 g, 34.8 mmol, 76% yleld) as a white solid.MS (M+H+): 397.11H NMR (400 MHz, CDCI3) delta [ppm]: 7.33-7.30 (t, J = 6Hz, 1 H), 7.27-7.24 (t, J = 6Hz, 1 H), 4.99 (s, 1 H), 4.57 (s, 1 H), 3.53-3.48 (m, 1 H), 3.33-3.28 (m, 1 H), 1 .62-1 .45 (q, 9H), 1.36-1.26 (m, 3H).

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.

1349718-98-4, name is 2,4-Dichloro-6-fluorobenzonitrile, 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. SDS of cas: 1349718-98-4

To a solution of 2,4-dichloro-6-fluorobenzonitrile (3.87 mmol) in 15 mL THF was added a solution of BH3 (15.5 mmol, 1M in THF) and the mixture was stirred at 60 C. for 1 h. After cooling to 0 C., water was added followed by MeOH and the mixture was then heated to 70 C. for 10 min. The solvent was evaporated, the residue was taken up in water and EtOAc. The aqueous phase was separated, basified with 1M NaOH and it was extracted 3 times with EtOAc. The combined organic layers were dried over MgSO4 and concentrated in vacuo to obtain the desired product as yellow oil. LC-MS (A): tR=0.39 min; [M+CH3CN+H]+: 234.90.

The synthetic route of 1349718-98-4 has been constantly updated, and we look forward to future research findings.

Related Products of 191014-55-8, The chemical industry reduces the impact on the environment during synthesis 191014-55-8, name is 4-Fluoro-2-methoxybenzonitrile, I believe this compound will play a more active role in future production and life.

General procedure: To a solution of (4S,5S)-4-hydroxy-5-methylpyrrolidin-2-one 7 33 (7.00 g, 60.8 mmol) in THF (120 mL) was added sodium bis(2-methoxyethoxy)aluminium dihydride (70% in toluene, 59.7 mL, 215 mmol) slowly at 5 C. After stirring at 70 C for 3 h, the reaction mixture was cooled to 5 C followed by addition of sodium carbonate decahydrate (26.1 g, 91.2 mmol). The mixture was stirred at room temperature for 16 h, diluted with THF, and the precipitate was filtered off. The filtrate was concentrated in vacuo, and the residue was dissolved in DMSO (80 mL). To the solution was added lithium carbonate (8.99 g, 122 mmol) and 2-chloro-4-fluorobenzonitrile (9.46 g, 60.9 mmol), and the mixture was stirred at 100 C for 1 h. The mixture was diluted with EtOAc and H2O, and the organic layer was dried over anhydrous MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane-EtOAc) to give 10 (10.7 g, 74%) as a colorless solid. 1H NMR (300 MHz, CDCl3) delta: 1.18 (3H, d, J = 6.6 Hz), 1.82 (1H, d, J = 5.5 Hz), 2.01-2.14 (1H, m), 2.25-2.35 (1H, m), 3.19-3.28 (1H, m), 3.43-3.51 (1H, m), 3.89-3.98 (1H, m), 4.43-4.52 (1H, m), 6.43 (1H, dd, J = 8.9 and 2.4 Hz), 6.56 (1H, d, J = 2.4 Hz), 7.42 (1H, d, J = 8.9 Hz). MS (ESI) m/z 237 [(M+H)+].

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-Fluoro-2-methoxybenzonitrile, other downstream synthetic routes, hurry up and to see.

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.