Author: Jessica.F

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. 16532-79-9, name is 4-Bromophenylacetonitrile, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Bromophenylacetonitrile

To a solution of 2-(4-bromophenyl)acetonitrile (2.00 g, 10.20 mmo) in THF (20 mL) was added NaH (1.22 g, 30.60 mmol, 60% purity) at 0 C. The mixture was stirred at 0 C for 30 mins, then Mel (4.34 g, 30.60 mmol, 1.90 mL, 3.00 eq) was added to the mixture. The mixture was stirred at 15 C for 16 hours. The mixture was quenched with sat.NH4Cl (50 mL) and extracted with EtOAc (50 mL x 2). The combined organic phase was washed with brine (20 mL), dried over Na2S04, filtered and concentrated to give the crude product that was purified by flash chromatography on silica gel (PE: EtOAc = 20:1 to 10:1) to afford A-73 (400.00 mg) as an oil. H NMR (400MHz, CDC13) _ = 7.53 (d, 2H), 7.36 (d, 2H), 1.72 (s, 6H).

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.

Application of 127667-01-0, 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 127667-01-0 as follows.

Preparation 27 5- Meth lox -1 /-/-indazol-3-amine 5-(Methyloxy)-1 H-indazol-3-amine: 2-Fluoro-5-(methyloxy)benzonitrile (5 g, 33.1 mmol) was dissolved in 1 -Butanol (50 mL), and hydrazine hydrate (20.61 mL, 662 mmol) was added. The reaction mixture was heated at 150 C for 48 hours then it was cooled to rt, diluted with water, and extracted with EtOAc (2×100 mL). The organic layer was washed with brine, dried over Na2S04 and concentrated under vacuum to give the title compound (2 g, 37%). 1H NMR (400 MHz, DMSO-cf6) delta ppm 3.75 (s, 3 H) 5.17 (s, 0 H) 6.89 (dd, J=9.03, 2.51 Hz, 0 H) 7.09 – 7.22 (m, 1 H) 1 1.18 (br. s., 7 H); MS (m/z) 164 (M+H+).

According to the analysis of related databases, 127667-01-0, 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. 623-03-0, name is 4-Chlorobenzonitrile, A new synthetic method of this compound is introduced below., name: 4-Chlorobenzonitrile

General procedure: A flask (25 mL) containing ruthenium(II) complex (1 M%) and 2-butanol (5 mL) was stirredfor 5 min under an argon atmosphere at room temperature. Afterwards, KOtBu(0.05 mM) was added and the mixture was stirred for another 5 min. Then, the nitrile(0.5 mM) was added and placed on a hot plate at 120 C for 30 min. After completion ofthe reaction, the catalyst was removed from the reaction mixture by addition of petroleumether followed by filtration and subsequent neutralization with 1 M HCl. The ether layerwas filtered through a short path of silica gel by column chromatography. To the filtrate,hexadecane was added as a standard and the yield was determined by GC.

The synthetic route of 623-03-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 3288-99-1, A common heterocyclic compound, 3288-99-1, name is 2-(4-(tert-Butyl)phenyl)acetonitrile, molecular formula is C12H15N, 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.

0.66 g (16.5 mmols) of sodium hydride and 2.6 g (15.0 mmols) of 4-tert-butylphenylacetonitrile were suspended in 50 ml of tetrahydrofuran. To the suspension was added dropwise 1.95 g (16.5 mmols) of dimethyl carbonate dissolved in 10 ml of tetrahydrofuran while stirring at room temperature. The mixture was refluxed with heating for 2 hours, and the solvent was distilled off under reduced pressure. Water was added to the residue, and the residue was acidified by diluted hydrochloric acid and twice extracted with 30 ml of ethyl acetate. The ethyl acetate extraction solutions were mixed, washed with a saturated brine solution, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. The residue thus-obtained was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1), giving 1.8 g of the desired product (yield 52%)

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.

1835-49-0, name is Tetrafluoroterephthalonitrile, 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. HPLC of Formula: C8F4N2

About 1.25 g (about 6.25 mmol) of the 1,4-dicyano-2,3,5,6-tetrafluorobenzene synthesized according to the procedure described in Example 1 was transferred into about 57.5 mL of N2 bubbled toluene, which was at about 0 C. About 17.5 ml (about 17.5 mmol) of 1 M DIBAL-H (diisopropylaluminumhydride) toluene solution was added. After the reaction mixture was stirred for about 2.5 hours at room temperature, the mixture was cooled to about 0 C.About 30 mL of about 2 N HCl was added until the pH of the mixture was less than about 2 units.The aqueous layer was then extracted several times with CH2Cl2.The organic layer was combined and dried by evaporation.The crude product was chromatographed with toluene as a carrier through silica gel and produced about 0.79 g of product (about 62%).The 1H NMR resonance of this product in CDCl3 was delta 10.36 and the 19F NMR resonance was delta -144.1 (singlet).The reaction scheme (5) is illustrated below.

The synthetic route of 1835-49-0 has been constantly updated, and we look forward to future research findings.

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. 85068-32-2, name is 2-(3,5-Bis(trifluoromethyl)phenyl)acetonitrile, A new synthetic method of this compound is introduced below., Quality Control of 2-(3,5-Bis(trifluoromethyl)phenyl)acetonitrile

[0156] 0.46 g (1.33 mmol) of the Nile-red compound derivative, 0.50 g (1.99 mmol) of 3,5-bis(trifluoromethyl)phenylacetonitrile, and 50 ml of acetic anhydride were placed in a 100 ml pear-shaped flask. The solution in the pear-shaped flask was heated in a silicone oil bath to 135 C. and allowed to react for 2 hours. Acetic anhydride was distilled off with an evaporator and the residue was dissolved in chloroform. This chloroform solution was washed with a 5% aqueous solution of sodium hydroxide and then with water. After the addition of sodium sulfate, the solution was allowed to stand for 30 minutes to be dried. The dried solution was concentrated with an evaporator. The obtained solid was purified by a column chromatography that used silica gel and benzene. 14 mg of violaceous solid was obtained. The melting point of the violaceous solid was 183-185 C. An NMR chart of this product is shown in FIG. 11. The results of elemental analysis of this violaceous product are as follows. Based on these results, the obtained product was identified as the Nile Red luminescent compound represented by formula (22). [0157] The results of elemental analysis [0158] Found values: C: 67.02, H: 4.77, N: 5.13 [0159] Calculated values: C: 66.90, H: 4.71, N: 5.03

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.

Related Products of 6575-12-8, A common heterocyclic compound, 6575-12-8, name is 2,6-Dibromobenzonitrile, molecular formula is C7H3Br2N, 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.

Embodiment 14 (S,E)-3-(4-((2-Hydroxymethylpyrrolidin-1-yl)methyl)-3,5-dimethoxystyryl)b iphenyl-2-carbonitrile 14 Synthesis of compound 14-c Phenylboronic acid (363mg, 3mmol) and 2,6-dibromobenzonitrile (783mg, 3mmol) were dissolved in a mixed solvent of 1,4-dioxane (20mL) and water (4mL), followed by addition of [1,1′-bis(diphenylphosphino)ferrocene]palladium dichloride dichloromethane complex (171mg, 0.21mmol) and sodium carbonate (1.06g, 10mmol). After the reaction system was purged three times with nitrogen, the reaction solution was heated to 80C and stirred for 16 hours. Then the reaction solution was cooled to room temperature and evaporated under reduced pressure. The residue was purified by silica gel column chromatography (petroleum ether) to give compound 14-c (280mg, yield 36%).

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 3215-64-3, 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. 3215-64-3, name is 2-(2,6-Dichlorophenyl)acetonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: A mixture of 15.3 g (100 mmol) of 2-(2,6difluorophenyl)acetonitrile, 152.5 g (70 mL, 812 mmol) of dibromoethane, and 32.7 g (144 mmol) of Et3BnN+Cl- was isolated from moisture and carbon dioxide and vigorously stirred at 60. A solution prepared from 95 g (1430 mmol, ?84.5%) of KOH and 95 mL of water was then added dropwise; the mixture was stirred during 6 h at 60-65C, and left overnight. On the next day, the reaction mixture was extracted with t-BuOMe (3×100 mL), the combined organic fractions were evaporated, and residual water was removed via azeotropic distillation with toluene. Then 60 mL of water and 40 mL of concentrated sulfuric acid were added to the obtained 1-(2,6-difluorophenyl)cyclopropanecarbonitrile, and the mixture was refluxed during 4 h. The reaction mass was cooled to ambient; the precipitate was filtered off and dried. Yield 17.82 g (90%), mp 156-157 (toluene).

The synthetic route of 2-(2,6-Dichlorophenyl)acetonitrile has been constantly updated, and we look forward to future research findings.

455-18-5, name is 4-(Trifluoromethyl)benzonitrile, 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. Formula: C8H4F3N

Step A (4-Trifluoromethylphenyl)thiocarboxamide To a stirred solution of 25.0 grams (0.146 mole) of 4-(trifluoromethyl)benzonitrile in 190 ml of pyridine was added 14.8 grams (0.146 mole) of triethylamine. During a two hour period, hydrogen sulfide gas was bubbled into the reaction mixture. The reaction mixture was stirred under a dry nitrogen atmosphere for 15 minutes and then was poured into ice-water. The aqueous mixture was extracted with three portions of diethyl ether. The organic extracts were combined and washed in succession with 10% hydrochloric acid, water, and an aqueous, saturated sodium chloride solution. The washed extract was dried over anhydrous sodium sulfate and was filtered. The filtrate was evaporated under reduced pressure to yield 28.3 grams of (4-trifluoromethylphenyl)thiocarboxamide as a solid.

The synthetic route of 455-18-5 has been constantly updated, and we look forward to future research findings.

Reference of 5332-06-9, The chemical industry reduces the impact on the environment during synthesis 5332-06-9, name is 4-Bromobutanenitrile, I believe this compound will play a more active role in future production and life.

Piperidine (3 equiv.) and toluene (5.5 volumes based on 4-bromobutanenitrile weight) were mixed and heated to 55-60 C. To this mixture, 4-bromobutanenitrile (1 equiv.) was added slowly while keeping temperature below 80 C. Note the addition is exothermic and the exotherm is addition-controlled. A white solid was observed to crystallize during the addition (piperidine hydrobromide). After complete addition, the reaction was stirred at 55-60 C. for an additional 1 hour. Progress of the reaction was monitored by 1H NMR in CDCl3 by sampling from the slurry, filtering, and evaporating solvent. After reaction is finished, the mixture was cooled to 10-20 C. and stirred for 1 hour. Solids were removed by filtration, and the cake washed with toluene (2×1.5 volumes based on 4-bromobutanenitrile weight). The combined filtrates were evaporated under vacuum (15-50 mmHg) at 40-50 C. until 120-200% of the theoretical weight was obtained. The solution was again filtered to remove remaining piperidine hydrobromide solids. The filtrate was then further evaporated under vacuum (15-50 mmHg) at 40-50 C. until no more solvent distilled. 1H NMR in CDCl3 was done to quantify residual amount of toluene for correction in next step and to verify that there was no residual piperidine present.

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