Month: April 2021

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.

Synthetic Route of 916792-13-7, These common heterocyclic compound, 916792-13-7, name is 4-Bromo-2-fluoro-5-methylbenzonitrile, 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: The requisite aryl boronate derivative was prepared from the corresponding aryl bromide via reaction with 4,4,4′,4′,5,5,5′,5′-octamethyl-2,2′-bi-l,3,2-dioxaborolane in the presence of [1,1′- bis(diphenylphosphino)ferrocene]dichloropalladium(l l) and potassium acetate.

The synthetic route of 916792-13-7 has been constantly updated, and we look forward to future research findings.

Related Products of 3047-38-9, 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. 3047-38-9 name is Cyclopent-1-enecarbonitrile, 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.

Step 1: 3-bromocyclopent-1-enecarbonitrile To a stirred solution of cyclopent-1-enecarbonitrile (50 g, 537 mmol) in tetrachloromethane (400 ml) at 25 C. was added was added N-bromosuccinimide (96 g, 537 mmol) under nitrogen atmosphere. The resulting mixture was refluxed for 2 h. The progress of reaction was monitored by TLC. The reaction mixture cooled to 25 C. and filtered through celite. The filtrate was concentrated under reduced pressure to obtain a crude product, which was purified by column chromatography over silica gel (100-200 mesh) using 1% ethyl acetate in hexane as an eluent to obtain the title compound (60 g, 65%). 1HNMR (CDCl3, 400 MHz): delta 6.77-6.73 (m, H), 5.12-5.09 (m, 1H) 2.95-2.86 (m, 1H) 2.67-2.42 (m, 3H)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Cyclopent-1-enecarbonitrile, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 5922-60-1, name is 2-Amino-5-chlorobenzonitrile, 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 5922-60-1, Formula: C7H5ClN2

Preparation 237N-(4-Chloro-2-cyanophenyl)-N-(methylsulfonyl)methanesulfonamide10726] To a solution of 2-amino-5-chloro-benzonitrile (5.00 g, 32.77 mmol) in pyridine (100 mE) at 0°C. was added methanesulphonylchloride (10.21 mE, 131.07 mmol) andthe reaction stirred at room temperature for 18 hours. The reaction was concentrated in vacuo and partitioned between 2N HC1 and EtOAc. The organic layer was collected, washed with brine, dried over sodium sulfate and concentrated in vacuo. The residue was triturated with 1:1 acetonitrile:ether to afford the title compound (8.00 g, 79percent).10727] ?H NMR (400 MHz, DMSO-d5): oe ppm 3.61 (s, 6H), 7.90 (d, 1H), 7.98 (dd, 1H), 8.31 (d, 1H).

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.

Synthetic Route of 7357-70-2,Some common heterocyclic compound, 7357-70-2, name is 2-Cyanothioacetamide, molecular formula is C3H4N2S, 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 stirred solution of 2-cyanothioacetamide (3.52 g, 35 mmol) and ethyl 2,4- dioxovalerate (5.0 g, 32 mmol) in anhydrous EtOH (75 mL) at room temperature was added triethylamine (0.5 mL) and the reaction was stirred overnight. Filtration and washing of the precipitates with EtOH gave [3-CYANO-2-MERCAPTO-6-METHYL-ISONICOTINIC] acid ethyl ester as a yellow solid (4.54 g, 64.5%). A mixture of this ester (3.54 g, 16 mmol), bromoacetamide (2.15 g, 16 mmol) and sodium ethoxide (2.18 g, 32 mmol) in MeOH was heated at reflux overnight. It was then allowed to cool to room temperature. Filtration and washing of the precipitates with EtOH provided 3-amino-2-carbamoyl-6- methyl-thieno [2, [3-B]] pyridine-4-carboxylic acid ethyl ester as a solid (0.94 g, 21. [1%).]

The synthetic route of 7357-70-2 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 42872-74-2 as follows. Safety of 3-Bromo-4-methylbenzonitrile

A solution of 3-bromo-4-methylbenzonitrile (1.0 g) in EtOH (20 mL) was saturated at 0 C. with gaseous HCl and the solution was stirred at rt for 2 h. The volatiles were removed under reduced pressure and the residue was dissolve in EtOH (9 mL). Formohydrazide (0.45 g) and triethylamine (2.8 mL) were added and the solution was stirred at 90 C. for 2 h. Water (50 mL) was added and the mixture was extracted with EtOAc. The combined organic layers were dried and the volatiles were removed under reduced pressure. The residue was purified by column chromatography (Interchim cartridge 30SiHP, 40 g, Cy/EtOAc) to yield the desired product (40% yield). LC-MS (Method 1): m/z [M+H]+=238.1 (MW calc.=238.08); Rt=3.3 min.

According to the analysis of related databases, 42872-74-2, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 65610-13-1, name is 3-Fluorophthalonitrile, 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. COA of Formula: C8H3FN2

A mixture of 3-fiuoro-l,2-cyanobenzene (2.49g), glycine ethyl ester hydrochloride(2.49g) and potassium carbonate (5.18g) in acetonitrile (25mL) was heated to reflux for24 hours. After cooling, the reaction mixture was extracted into dichloromethane, washedwith water, dried (MgSCU) and the solvent removed hi vacuo to yield crude productwhich was purified using flash chromatography to yield (2,3-dicyano-phenylamino)-acetic acid ethyl ester (840mg).A mixture of (2,3-dicyano-phenylamino)-acetic acid ethyl ester (453mg), triethylamine(0.24mL), di-tert-butyl dicarbonate (447mg) and 4-ditnethylaminopyridine (20mg) wasstirred in dichloromethane (5mL) at room temperature overnight. The reaction mixturewas then extracted into dichloromethane, washed with water, dried (MgSO4) and thesolvent removed in vacuo to yield crude product which was purified using flashchromatography to yield the title compound (606mg).

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