Author: Jessica.F

Related Products of 110882-60-5, 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. 110882-60-5 name is 3-Fluoro-5-nitrobenzonitrile, 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 1; Step 2 To solution of 1.0 eq 1B in dry Et2O (0.06 M) at 0 C. was added dropwise a solution of diisobutyllithiumaluminum hydride (1.1 eq, 1.0 M in hexanes) by syringe. The resulting solution was kept at 0 C. overnight. The reaction mixture was added to a mixture of ice and glacial acetic acid. The reaction mixture was then diluted with ethyl acetate, and the aqueous layer was extracted with ethyl acetate two additional times. The combined organic layers were washed twice with saturated sodium bicarbonate, and once with brine. The organic layers were then dried over sodium sulfate, filtered and concentrated in vacuo. Purification over silica gel using 10% EtOAc/hexanes as the eluant afforded a yellow solid (100%) as an 80:20 mixture of 1C:1B.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Fluoro-5-nitrobenzonitrile, and friends who are interested can also refer to 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. 75344-77-3, name is 4-Bromo-3,5-dimethylbenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-3,5-dimethylbenzonitrile

Example 2; Preparation of (S)-2-tert-Butoxvcarbonvlamino-3-(4-cvano-2,6-dimethvl- phenvD-propionic acid methyl esterA 5OmL three-necked round bottom flask equipped with an addition funnel, magnetic stirrer, heating mantel, and thermocouple was charged under nitrogen dry DMAc (2mL), I2 (38.1 mg, 0.15mmol) and zinc powder activated (washed with 10% HCI, rinsed with H2O and acetone) (393 mg, 6 mmol). The resulting mixture was stirred at 23C until the red color of I2 disappeared (2 minutes). A solution of Boc-beta-iodo-L-alanine methyl ester (1 g, 3mmol) in DMAc (2 ml.) was added slowly, (temperature change from 210C to 29C) and the resulting mixture was stirred at 8O0C for 0.5-1 hour, then co cooled to 35C. To the resulting mixture were added, successively, 4-bromo-3,5-dimethyl- benzonithle (315 mg, 1.5mmol) in DMAc (6ml_), P(o-tol)3 (36.5 mg, 0.12 mmol) and Pd2(dba)3 (55 mg, O.Odeltammol). The resulting mixture was heated to 700C, with stirring for 1 hour, then cooled to ambient temperature. The resulting mixture was diluted with EtOAc (15ml_) and filtered with STAND SUPER-CEL 815520. The EtOAc solution was quenched with 1 N HCI (4OmL) and extracted with ethyl acetate (2OmL). The combined organic phases were washed with H2O (2 x 5OmL) and then with 50% brine, dried over Na2SO4 , filtered and evaporated to dryness in vacuo to yield a brown solid. The title compound was crystallized from EtOAc (5mL) and heptane (4OmL) to yield a white solid.

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.

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. 31643-49-9, name is 4-Nitrophthalonitrile, This compound has unique chemical properties. The synthetic route is as follows., category: nitriles-buliding-blocks

General procedure: 4-Nitrophthalonitrile (1mmol) 1, hydroxy compound (2mmol) 2 or 7 and dry potassium carbonate (8mmol) were dissolved in 50mL dry DMSO and stirred at room temperature under nitrogen for 48h. The reaction mixture was poured into 200mL distilled water and stirred for 15min. The crude product was recovered by filtration and washed with water. The residue was recrystallized from methanol/water mixture 1:1 and dried under vacuum.

According to the analysis of related databases, 31643-49-9, 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. 36282-26-5, name is 2-Bromo-4-fluorobenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C7H3BrFN

4-Fluoro-2-(2-oxooxazolidin-3-yl)bejizonitrile. A 48 mL pressure vessel containing 2-bromo-4-fluorobenzonitrile (1.00 g, 5.00 mmol), 2-oxazolidone (0.390 g, 4.50 mmol), K2CO3 (0.970 g, 7.0 mmol) and xantphos (0.231 g, 0.40 mmol) in dioxane (10 mL) was degassed with argon for 15 min. Pd2dba3 (0.140 g, 0.15 mmol) was introduced and then the reaction mixture was heated at 70 0C for 18 h. The mixture was cooled, diluted with dioxane, and then filtered through Celite. The resulting mixture was concentrated in vacuo and subjected to column chromatography on silica gel with hexanes-.ethyl acetate (1:1) to (3:7) gradient as the eluent to afford the title compound as a white solid (0.460 g, 50% yield): 1H NMR (400 MHz, CDCl3) delta ppm: 7.73 (IH, dd, J = 5.8, 8.6 Hz), 7.43 (IH, dd, J = 2.5, 9.6 Hz), 7.11 (IH, ddd, J = 2.5, 7.5, 8.7 Hz), 4.60 (2H, t, J = 7.1 Hz), 4.29 (2H, t, J = 7.1 HJz); LCMS f ESI, M+H*) m/z 207.

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.

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. 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C8Cl4N2

Under nitrogen gas, 4,5-dichlorophthalonitrile (5.0 mmol), Ethyl vanillate (7.5 mmol), K2CO3 (50.0 mmol) was dissolved in 30 ml of anhydrous DMF and refluxed at 100 for 12 hours. When the reaction was complete, the reaction solution was slowly dropped on ice-water in a dropwise manner. The precipitate was filtered off under reduced pressure, washed with distilled water, and the dried crude product was purified by column chromatography (eluent: MC: MeOH = 15: 1)

According to the analysis of related databases, 1953-99-7, 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. 17417-09-3, name is 2-Fluoro-5-nitrobenzonitrile, A new synthetic method of this compound is introduced below., Quality Control of 2-Fluoro-5-nitrobenzonitrile

A solution of 2-fluoro-5-nitro-bezonitrile (300 mg, 1.81 mmol) and methyl hydrazine (170 mg, 3.62 mmol) in dioxane (10 mL) was stirred at 80 C. for 2 h. The reaction mixture was cooled and partitioned between 1N aqueous HCl and EtOAc. The organic layer was washed with water dried over Na2SO4 filtered and concentrated to the desired product 5-nitro-1-methyl-1H-indazol-3-ylamine (280 mg, 80%). HRMS for C8H8N4O2 (M+H) calcd: 193.0720. Found:193.0720

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. 105-34-0, name is Methyl 2-cyanoacetate, A new synthetic method of this compound is introduced below., name: Methyl 2-cyanoacetate

1-nitro-naphthalene (97 g, 0.56 mol), methyl cyanoacetate (166.5 g, 1.68 mol), potassium cyanide (40.1 g, 0.62mol), potassium hydroxide (62.9 g, 1.12 mol) and dissolved in dimethylformamide (970 mL) and the mixture was stirred overnight at 60C. After concentrated under reduced pressure to remove the solvent at room temperature into a 500 mL 10% aqueous sodium hydroxide solution was refluxed for about one hour. After extraction with ethyl acetate and separated by column chromatography and recrystallized from toluene-heptane to give the Sub 2-2-1 50.8 g (yield: 54%).

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.

Synthetic Route of 60702-69-4, 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. 60702-69-4, name is 2-Chloro-4-fluorobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 11 2-Chloro-4-(3-endo-hydroxy-8-azabicyclo[3.2.1]oct-8-yl)-3-iodobenzonitrile (195JP18) Adapting a protocol by Uchiyama et al (J. Am. Chem. Soc., 2002, 124, 8514-8515), which reference is incorporated herein by reference in its entirety, 2-chloro-4-fluorobenzonitrile (311 mg, 2.0 mmol) in dry THF (1.0 mL) was added dropwise to lithium di-t-butyl(2,2,6,6-tetramethylpiperidino)zinncate (4.0 mmol in 10 mL THF, Uchiyama et al J. Am. Chem. Soc., 1999, 121, 3539-3540, which is incorporated herein by reference in its entirety) at 0 C. and stirred at 0 C. for 3.5 h. Iodine (5.08 g, 20.0 mmol) was then added and the reaction was stirred at r.t. overnight. Na2S2O3 (1.0 M, 50 mL) and saturated aqueous NH4Cl (100 mL) were added, followed by extraction with dichloromethane (3*100 mL), drying of the combined organic layers over Na2SO4, filtering, and removal of the solvents in vacuo. The residue was passed through a pad of silica gel eluding with EtOAc/n-heptane (1:40), affording 112 mg (0.40 mmol) of 2-chloro-4-fluoro-3-iodobenzonitrile. This material was combined with nortropine (114 mg, 0.90 mmol), K2CO3 (186 mg, 0.134 mol) and DMSO (2.0 mL), and stirred at 130 C. for 1.5 h. The crude mixture thus obtained was diluted with n-heptane (10 mL), passed through a pad of silica gel using EtOAc/n-heptane (1:2), concentrated and purified by preparative TLC (EtOAC/n-heptane, 1:1) to give 1.5 mg (1.7%) of 195JP18 as an off-white solid. Rf=0.21 (EtOAc/n-heptane 1:1). LC/MS m/z 389 [M+H]+. 1H-NMR (CDCl3) delta 7.42 (d, 1H, J=8.6), 6.70 (d, 1H, J=8.6), 4.16 (br s, 1H), 3.95 (br s, 2H), 2.50-2.22 (m, 4H) 1.93-1.78 (m, 4H).

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-4-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Reference of 1953-99-7,Some common heterocyclic compound, 1953-99-7, name is 3,4,5,6-Tetrachlorobenzene-1,2-dicarbonitrile, molecular formula is C8Cl4N2, 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.

With molar ratio: tetrachlorophthalonitrile, anhydrous potassium fluoride, N, N-dimethylformamide = 1.0: 4.0: 20.Tetrachlorophthalic phthalonitrile, anhydrous potassium fluoride, N, N-dimethylformamide into chemical reactor, with stirring by increasing the temperature tetrachloro phthalonitrile, anhydrous potassium fluoride was dissolved in N, N-dimethylformamide and the temperature was raised to 110 , maintaining this temperature for 7 hours the stirring was stopped after the reaction, cooling to room temperature, to obtain a liquid mixture; chemical reactor a liquid mixture in a distillation column, the distillate is tetrafluorophthalonitrile, forthwith fed into the dryer, drying at a temperature of 60 for 2.0 hours and then was fed into the drying mill, pulverized into a powder that is finished.

The synthetic route of 1953-99-7 has been constantly updated, and we look forward to future research findings.

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 36282-26-5 as follows. Computed Properties of C7H3BrFN

2-(Benzofuran~2-yl)~4-fluorobenzonitriIe (AUPOl 158-1)A mixture of 2-bromo-4-fluorobenzonitrile (5,15 g, 25.65 mmol), benzofuran-2- ylboronic acid (5.0 g, 30,8 mmol), 1 ,2-dimethoxyethane (25 mL) and 2M Na2CO3 (40 niL) was heated to reflux before Pd2(dba)3 (100 mg) was added and heating was continued for 5 h. After cooling to r.t, EtOAc (20 mL) was added to dissolve the product. The mixture was filtered through celite, the organic layer was separated, dried (Na2SO4) and concentrated under reduced pressure, The residue was dissolved in minimum amount of CHCl3 and passed through Silica. Solvent was evaporated and the residue was first purified by crystallisation from a mixture CHCI3/PE (98/2). The filtrate was purified by Combiflash chromatography (40 g column, 13 g Silica, gradient of eluent from PE to PE/EtOac 9/1) to give the title compound as light yellow solid purified by rinsing with PE to give at the end a white solid (5.15 g), This solid had to be purified an ultimate time by drying under vacuum at 80 0C for O/N. Finally, pure expected compound was obtained as a off-white solid in 59% yield (3.6 g); mp 123-124 0C; 1H NMR (270 MHz, CDCl3) .57.13 (IH, td, J = 2.5 and 7.3 Hz, ArH), 730 (IH, X, J = 1.1 Hz5 ArH), 7,40 (IH, X, J = 1.1 Hz, ArH), 7.56 (IH5 d, J = 7.7 Hz, ArH), 7,69 (IH, d, J = 7.7 Hz, ArH), 7.76-7.86 (3H, m, ArH); Anal. Calcd. for Ci5H8FNO: C 75,94, H 3.40, N 5.90. Found: C 75,70, H 3.37, N 5.97 %.

According to the analysis of related databases, 36282-26-5, the application of this compound in the production field has become more and more popular.