Month: May 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. 175596-01-7, name is Methyl 4-cyano-2-fluorobenzoate, A new synthetic method of this compound is introduced below., COA of Formula: C9H6FNO2

Step 2: methyl 4-[amino(hydroxyimino)methyl]-2-fluorobenzoate To a solution of methyl 4-cyano-2-fluorobenzoate, obtained in Step 1 (486.8 mg; 2.72 mmol) in abs. EtOH (6 ml_) was added hydroxylamine (0.8 ml 13.6 mmol; 5 eq.) (50% in water) and the mixture was heated at 74C overnight. After cooling, a product precipitated. The precipitate was filtered off and dried under vacuum to afford Intermediate 1 as an off-white solid (267.10 mg; 46%). 1H-NMR (DMSO-d6, 300MHz) delta 10.09 (s, 1 H), 7.92 (t, J = 7.91 Hz, 1 H), 7.69 (dd, J = 1.70 Hz, J = 8.10 Hz, 1 H), 7.64 (dd, J = 1.51 , J = 12.81 , 1 H), 6.05 (s, 2H), 3.90 (s, 3H). HPLC (Method B) Rt 2.99 min (Purity: 100%).

The synthetic route of 175596-01-7 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. 96606-37-0, name is 2,4,6-Trifluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H2F3N

In one embodiment,The 6 mmol of the second reactant was dissolved in 15 ml to 25 ml of the first solvent tetrahydrofuran, and then 0.5 mmol to 2 mmol of the first additive sodium hydride was slowly added.The reaction is carried out for 20-50 minutes under room temperature conditions and under nitrogen.Then add 2 mmol of the first reactant and continue the reaction for 12 hoursTo obtain a mixture including the electroluminescent material.The mixture of the electroluminescent material is cooled to room temperature and poured into distilled water.Extraction with a first extraction solvent, and then washing with a first detergent,Drying with a first desiccant, and then performing chromatography,Obtain the first crude product, and then use the first eluent to obtain the electroluminescent material, and the electroluminescent material is a white solid,The yield was 64%.

According to the analysis of related databases, 96606-37-0, the application of this compound in the production field has become more and more popular.

Reference of 57381-49-4, 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 57381-49-4 as follows.

Into a 19-mL sealed tube was placed 2-bromo-4-chlorobenzonitrile (216 mg, 1.00 mmol), dioxane (1.5 mL), water (0.3 mL), Pd(dppf)Cl2 (36 mg, 0.05 mmol), Na2CO3 (318 mg, 2.97 mmol), and phenylboronic acid (148 mg, 1.21 mmol). The resulting solution was stirred for 16 h at 95oC. The reaction was then quenched by the addition of 25 mL of water. The resulting solution was extracted with ethyl acetate (3×15 mL) and the organic layers were combined. The organic layer was washed with brine (25 mL), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated under vacuum. The residue purified via a silica gel chromatography with ethyl acetate/petroleum ether (1:20). This resulted in 50 mg (23% yield) of 4-chloro-2-phenylbenzonitrile as a white solid.1H NMR (400 MHz, DMSO-d6, ppm): delta 8.00 (d, J = 8.4 Hz, 1H), 7.74 (d, J = 2.1 Hz, 1H), 7.68 (dd, J = 8.3, 2.2 Hz, 1H), 7.65 – 7.59 (m, 2H), 7.58- 7.48 (m, 3H), 4.04 (dd, J = 1.9, 1.0 Hz,1H).

According to the analysis of related databases, 57381-49-4, the application of this compound in the production field has become more and more popular.

Application of 69395-13-7, These common heterocyclic compound, 69395-13-7, name is 4-(2-Hydroxyethyl)benzonitrile, 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.

Step A Preparation of 4-(2-hydroxyethyl)benzylamine A solution of 0.74 g (0.005 mol) of p-cyanophenethyl alcohol in 50 ml of ethanol containing 10 ml of concentrated hydrochloric acid was hydrogenated at 30 psi using 0.1 g 5% Pd/C for 72 hours. The catalyst was removed by filtration and the solvent was removed under reduced pressure.

Statistics shows that 4-(2-Hydroxyethyl)benzonitrile is playing an increasingly important role. we look forward to future research findings about 69395-13-7.

Related Products of 6136-93-2,Some common heterocyclic compound, 6136-93-2, name is 2,2-Diethoxyacetonitrile, molecular formula is C6H11NO2, 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 solution of diethoxyacetonitrile (1 ,120 g, 930 mmol) in MeOH (500 ml_) was added a 17% solution of (NH4)2S in H20 (440 ml_) at rt. The mixture was stirred at rt overnight. The mixture was evaporated in vacuo to approximately 100 ml_ volume and filtered. The solid was washed with cooled water and dried in vacuo to afford the title compound 2 (92 g, 61 %) as a white solid, which was used as such in next step.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,2-Diethoxyacetonitrile, its application will become more common.

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. 425379-16-4, name is 2-Bromo-3-fluorobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C7H3BrFN

(4aS,5S)-1-(4-Fluorophenyl)-4a-methyl-5-[2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)ethyl]-1,4,4a,5,6,7-hexahydrocyclopenta[f]indazol-5-ol (13) (200 mg, 0.456 mmol), 2-bromo-3-fluorobenzonitrile (91 mg, 0.456 mmol), 1,1′-bis(di-tert-butylphosphino)ferrocene palladium dichloride (30 mg, 0.046 mmol), and Cs2CO3 (446 mg, 1.37 mmol) in degassed toluene(0.9 mL)/water (0.3 mL) were heated at 80 C for 1 h. The reaction was quenched with water and extracted with EtOAc (×3). The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography on Silica, eluting with a gradient of 0-100% EtOAc in hexanes to afford 14 (139 mg, 71%) as a white solid; 1H NMR (CDCl3, 500 MHz): delta 7.50 (s, 1H), 7.44-7.40 (m, 3H), 7.33-7.25 (m, 2H), 7.17 (t, J = 8.3 Hz, 2H), 6.15 (s, 1H), 3.18 (td, J = 12.7, 4.5 Hz, 1H), 2.97 (td, J = 12.6, 4.8 Hz, 1H), 2.84 (d, J = 15.4 Hz, 1H), 2.65 (dd, J = 19.0, 9.8 Hz, 1H), 2.53-2.42 (m, 2H), 2.34-2.26 (m, 1H), 2.07-1.98 (m, 1H), 1.88-1.80 (m, 1H), 1.75-1.67 (m, 1H), 1.17 (s, 3H), 0.90-0.82 (m, 1H); MS (ESI): m/z = 432.09 (MH+), 100% pure by LC-MS.

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 425379-16-4.

Some common heterocyclic compound, 120351-94-2, name is 3-(2-Aminoethoxy)benzonitrile, molecular formula is C9H10N2O, 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. Quality Control of 3-(2-Aminoethoxy)benzonitrile

Example 27 Synthesis of N-[2-(3-amidinophenoxy)ethyl]-3-(2-aminoethoxy)benzamidine tristrifluoroacetate: 10 ml of ethanol containing 30 % (w/v) of hydrogen chloride was added to 1.75 g (8.84 mmol) of 3-(2-aminoethoxy)benzonitrile, and the resultant mixture was stirred at room temperature for 22 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in 10 ml of 10 % (w/v) solution of ammonia in ethanol. The obtained solution was stirred at room temperature for 31 hours. The solvent was evaporated, and the obtained residue was purified by the reversed-phase high-performance liquid chromatography with silica gel, containing octadodecyl group chemically bonded thereto, as the filler. After the elution with a mixed solvent of water and acetonitrile containing 0.1 % (v/v) of trifluoroacetic acid, the fraction of the intended product was freeze-dried to obtain the title compound. Yield: 134 mg (0.195 mmol) (2.2 %). MS (ESI, m/z) 342 (MH+) H-NMR (DMSO-d6) delta 3.20-3.23 (2H, m), 3.81-3.85 (2H, t), 4.24 (2H, dd), 4.38 (2H, dd), 7.25-7.40 (4H, m), 7.50-7.60 (4H, m), 8.18 (2H, brs), 9.60 (4H, t).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 120351-94-2, its application will become more common.

Reference of 22364-68-7, 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. 22364-68-7, name is 2-(o-Tolyl)acetonitrile, This compound has unique chemical properties. The synthetic route is as follows.

Part A Preparation of ethyl 2-(alpha-cyano-2′-methylphenylacetyl)cyclohexyl carboxylate Using the procedure described in Example I, Part A, and starting with 159.80 g (0.700 mol) of diethyl 1,2-cyclohexanedicarboxylate, 61.65 g (0.47 mol) of 2-methylbenzyl cyanide, 14.06 g (0.61 mol) of sodium, and 250 ml of ethanol, 87.74 g (60% yield) of the desired cyano keto ester was obtained as a red, viscous oil.

The chemical industry reduces the impact on the environment during synthesis 2-(o-Tolyl)acetonitrile. I believe this compound will play a more active role in future production and life.

Application of 868-54-2,Some common heterocyclic compound, 868-54-2, name is 2-Aminoprop-1-ene-1,1,3-tricarbonitrile, molecular formula is C6H4N4, 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: Heterocyclic ketene aminals (1 mmol), aryl aldehydes (1.2 mmol), malononitriledimer (1.5 mmol), acetic acid (1 mmol), piperidine (1 mmol) and ethanol (10 mL)were stirred at refluxing for 1 h. After completion of the reaction (confirmed by TLC),the reaction mixture was filtered to afford the crude product, which was furtherwashed with 95% ethanol to give pure product 4.

The synthetic route of 868-54-2 has been constantly updated, and we look forward to future research findings.

Electric Literature of 134450-56-9, These common heterocyclic compound, 134450-56-9, name is 4,5-Difluorophthalonitrile, 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: A solution of 5a (67 mg, 0.61 mmols) in DMF (10 mL) was treated NaH (60 %, 48mg, 1.2 mmols), allowed to stir for half a minute at room temperature followed by addition of phthalonitrile 6 (100 mg, 0.61 mmols). A deep blue coloration developed in the reaction flask and TLC monitoring in 10 minutes showed complete consumption of both starting materials 5a and 6 and appearance of a new spot more non-polar to both starting materials, which was very strongly UV-active. The reaction was quenched in cold water (100 mL), extracted into ethyl acetate (20 mL), organic layer repeatedly washed with brine solution (5 × 15 mL) and dried over sodium sulfate. Evaporation of the majority of ethyl acetate followed by re-crystallization in an ice-bath yielded 7a (single spot by TLC control, 30% Ethyl acetate/Petroleum ether) as buff-colored crystals. Yield (62 mg, 43%). 1H NMR (300 MHz, d6-DMSO): delta 7.82 (s, 2H), 7.05 (s, 4H); 13C NMR (150 MHz, d6-DMSO): delta 145.57, 140.06, 125.67, 121.99, 116.76, 115.27, 110.81; UV-vis (DMSO) lambdamax (log epsilon) 261 (4.53), 324 (3.48); HRMS (ESI+) calcd. for C14H6N2O2Na 257.0327, observed for C14H6N2O2Na 257.0293. Melting point: 311 C.

Statistics shows that 4,5-Difluorophthalonitrile is playing an increasingly important role. we look forward to future research findings about 134450-56-9.