Category: nitriles-buliding-blocks

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 22972-63-0 as follows. category: nitriles-buliding-blocks

A solution of DIBAL ([1 M] in toluene) (1 60.9 ml_, 160.9 mmol, 2.5 eq) was added dropwise to a stirred solution of 2-(3,5-Dimethoxy-phenyl)-2-methyl-propionitrile (13.2 g, 64.36 mmol, 1 eq) in dry CH2CI2 (320 ml_) under nitrogen at -78 SC. The reaction mixture was stirred at -78 SC for 1 h. An aqueous solution of potassium sodium tartrate (10% solution in water) was added dropwise and the reaction mixture was warmed to room temperature and stirred vigorously overnight. The solid was filtered through celite and rinsed with CH2CI2, the product was extracted with CH2CI2. The combined organic layers were washed with brine and water, dried over anhydrous MgSC , filtered and the solvent was removed under reduced pressure. The product was purified by chromatography on silica gel (heptane/EtOAc, from 100:0 to 80:20). The desired fractions were collected and concentrated to afford the title product as a colorless oil. (1 1 .6 g, 86.5 %). 1 H NMR (300 MHz, CDC ) d 9.46 (s, 1 H), 6.40 (s, 3H), 3.79 (s, 6H), 1 .43 (s, 6H). LC-MS (ESI+): 209.1 (M+H+); R.T. : 1 .388 min. (HPLC Method E).

According to the analysis of related databases, 22972-63-0, the application of this compound in the production field has become more and more popular.

185836-35-5, name is 4-(Benzyloxy)-2-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. COA of Formula: C14H10FNO

Preparation 26 tert-butyl (3R,4S)-4-(5-(benzyloxy)-2-cvanophenoxy)-3-fluoropiperidine-1-carboxylate To a solution of 4-(benzyloxy)-2-fluorobenzonitrile (WO2006016548, 1 g, 4.4 mmol) in DMF (20 ml_) was added tert-butyl-(3R,4S)-3-fluoro-4-hydroxypiperidine (JOC (2013), 78 (17), 8892-8897, 1 g, 4.84 mmol) and cesium carbonate (2.86 g, 8.802 mmol). The reaction was heated to 100C for 16 hours before cooling and diluting with EtOAc. The solution was washed with water, brine, dried over sodium sulphate and concentrated in vacuo. The residue was purified using silica gel column chromatography eluting with 10% EtOAc in hexanes to afford the title compound as a yellow gum (1.7 g, 90%). 1 H NMR (400 MHz, DMSO-d6):5 ppm 1.40 (s, 9H), 1 .70-1.90 (m, 2H), 2.95-3.40 (m, 2H), 3.80-3.90 (m, 1 H), 4.00-4.15 (m, 1 H), 4.86-5.00 (m, 2H), 5.19 (s, 2H), 6.77-6.79 (m, 1 H), 6.99 (s, 1 H), 7.34-7.47 (m, 5H), 7.65-7.67 (m, 1 H). MS m/z 427 [M+H]+

The synthetic route of 185836-35-5 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. 3759-28-2, name is 2-(Cyanomethyl)benzonitrile, A new synthetic method of this compound is introduced below., Product Details of 3759-28-2

General procedure: A well stirred solution of the base aromatic amine (0.01 mol) in 2 N hydrochloric acid (15 mL) was cooled in an ice-salt bath and diazotized with sodium nitrite (0.01 mol) in water (5 mL). The mixture was then tested for complete diazotization using starch iodide paper which gives a weak blue test. If the mixture does not give the test, more sodium nitrite was added dropwise until a positive test is obtained and the color is stable for few minutes. If, on the other hand, strong test for nitrite is obtained, a few drops of a dilute solution of the base hydrochloride are added until the nitrite test is nearly negative. The above cold diazonium solution was added slowly to a well stirred solution of compound 1 (1.42 g, 0.01 mol) in ethanol (20 mL) containing sodium acetate (1 g) and the mixture was cooled in an ice-salt bath. After the addition of the diazonium salt solution, the reaction was tested for coupling reaction. A drop of the reaction mixture was placed on a filter paper and the colorless ring surrounding the spot dye was treated with a drop of an alkaline solution of a reactive coupler, such as a sodium salt of 3-hydroxy-2-naphthanilide. If unreacted diazonium salt is present, a dye is formed. The presence of unreacted coupler can be determined in a similar manner using a diazonium salt solution to test the colorless ring. After the coupling reaction was complete, the reaction mixture was stirred for 15 min at room temperature to coagulate the dye particles. The precipitated deep-colored product formed was filtered off, washed with water several times, dried and crystallized from dioxane to give compounds 2a-e.

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. 38487-86-4, name is 2-Amino-4-chlorobenzonitrile, A new synthetic method of this compound is introduced below., COA of Formula: C7H5ClN2

3-phenylpropiolic acid(185 mg, 1.27 mmol) was suspended in dichloromethane (1.9 ml), there to oxalyl chloride (0.114 ml, 1.33 mmol), and stirred for 2 hours at room temperature was added a DMF (1 drop). Thereto 2-amino-4-chlorobenzonitrile (194 mg, 1.27 mmol) and stirred overnight at room temperature added. After the reaction, water was added. Through a diatomaceous earth column (VARIAN Chem Elute 12198006), it was washed with chloroform. The solvent was distilled off and the residue was purified by silica gel column chromatography (SNAP 25 g, hexane / ethyl acetate) to give the title compound (268 mg, 75.2%) as a pale yellow 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.

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.

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.

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.

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.

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. 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.