Author: Jessica.F

Application of 621-03-4,Some common heterocyclic compound, 621-03-4, name is 2-Cyano-N-phenylacetamide, molecular formula is C9H8N2O, 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: To a solution of NaOEt (3.0 mmol) in anhydrous ethanol (10 mL) were added amide (2.0 mmol) and 2-aryl vinamidinium salt (2.0 mmol) at room temperature. The reaction mixture was stirred at the same temperature for 24 h. After completion of the reaction, the reaction mixture was poured into water (100 mL) to precipitatethe crude product, which was collected by filtration and washed with water. The residue was purified by silica gel column chromatography(CH2Cl2:MeOH) to afford the corresponding 1,5-diarylpyridin-2(1H)-one.

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

Electric Literature of 29509-06-6,Some common heterocyclic compound, 29509-06-6, name is 4-Methyl-3-oxopentanenitrile, molecular formula is C6H9NO, 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.

Example B22 To a stirring suspension of 6-aminobenzothiazole (0.500 g, 3.33 mmol) in cone. HCl (5 ml) at 0-5 C. was added a solution of NaNO2 (0.276 g, 3.99 mmol) in H2O (5 ml). The mixture was stirred at 0-5 C. for 75 min until a clear yellow solution was obtained. To this was then added a solution of SnCl2.2H2O (2.76 g, 13.3 mmol) in conc. HCl (5 ml). After completing the addition, the suspension was stirred at RT for 2 h. 4-Methyl-3-oxopentanenitrile (0.444 g, 3.99 mmol) and EtOH (50 ml) were added and the reaction was stirred with heating at 75 C. After 18 h, the completed reaction was cooled to RT and concentrated to an aqueous residue. This was chilled thoroughly in ice and made strongly basic (pH 12-13) by the addition of 6M NaOH. While still cold the mixture was extracted with EtOAc (2*). The combined organics were washed with H2O (2*), brine (1*), dried (MgSO4), filtered and evaporated to afford crude 1-(benzo[d]thiazol-6-yl)-3-isopropyl-1H-pyrazol-5-amine (0.8 g, 93% yield) as an oil which was used as is in the next reaction. 1H NMR (400 MHz, DMSO-d6) delta 9.36 (s, 1H), 8.30 (d, J=2.4 Hz, 1H); 8.10 (d, J=8.8 Hz, 1H), 7.74 (dd, J=2.4 and 8.8 Hz, 1H), 5.36 (s, 1H), 5.33 (brs, 2H), 2.76 (septet, J=6.8 Hz, 1H), 1.17 (d, J=6.8 Hz, 6H); MS (ESI) m/z: 259.0 (M+H+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4-Methyl-3-oxopentanenitrile, its application will become more common.

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. 21524-39-0, name is 2,3-Difluorobenzonitrile, A new synthetic method of this compound is introduced below., Recommanded Product: 2,3-Difluorobenzonitrile

To a solution of 7-hydroxy-2-(4-(1-methyl-1H-pyrazol-9-yl}benzyl)isoindolin-1-one (0.050 g) obtained in Reference Example 6 in DMF (2 mL) was added potassium tert-butoxide (0.018 g), and the mixture was stirred under an argon atmosphere at room temperature for 30 min. To the reaction solution was added 2,3-difluorobenzonitrile (0.024 g), and the mixture was stirred at 50C for 6 hr. The reaction mixture was diluted with ethyl acetate, and washed with saturated brine. The organic layer was separated, dried over anhydrous sodium sulfate, and concentrated. The residue was crudely purified by NH silica gel chromatography (hexane-ethyl acetate), and solidified with hexane-ethyl acetate to give the title compound (0.035 g). MS: [M+H]+ 439.2 1H NMR (400 MHz, DMSO-d6) 5 3.85 (3H, s), 4.41 (2H, s), 4.66 (2H, s), 6.84 (1H, d, J = 8.3 Hz), 7.27 (2H, d, J = 8.1 Hz), 7.33 (1H, d, J = 7.3 Hz), 7.46-7.58 (4H, m), 7.77-7.86 (3H, m), 8.12 (1H, s).

The synthetic route of 21524-39-0 has been constantly updated, and we look forward to future research findings.

Electric Literature of 50397-74-5, 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. 50397-74-5, name is 4-Amino-3-bromobenzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 1 :- Preperation of (E)-methyl 3-(2-amino-5-cyanophenyl)acrylate To a mixture of 4-amino-3-bromobenzonitrile (10.0 g, 0.050 mmol) and methyl acrylate (9.19 mL, 0.101 mmol) in acetonitrile (200 mL) was added palladium acetate (0.568 g, 0.0025 mmol) and tri-o-tolyl phosphine (1.54 g, 0.005 mmol) and Et3N (14.64 mL, 0.105 mmol). The reaction mixture was heated to reflux for 48 h. The reaction mass was filtered through celite and washed the bed with ethyl acetate. The filtrate was concentrated to afford 6.0 g of title product. 1H NMR (300 MHz, DMSO): delta 7.92 (s, 1H), 7.82-7.77 (d, = 15.6 Hz, 1H), 7.41-7.38 (d, = 8.7 Hz, 1H), 6.77- 6.74(d, = 8.7 Hz, 1H), 6.64 (s, 2H), 6.56-6.51 (d, = 15.6 Hz, 1H), 3.70 (s, 3H).

The synthetic route of 4-Amino-3-bromobenzonitrile has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 302912-31-8, name is Ethyl 2-(4-cyanophenyl)-2-oxoacetate, 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. Product Details of 302912-31-8

To a solution of ethyl (4-cyanophenyl)(oxo)acetate (5.0 g, 24.6 mmol) in water (100 mL) was added concentrated hydrochloric acid (100 mL). The solution was heated to reflux for 16 hours. The solution was cooled to ambient temperature and the solids were filtered and dried to give 4- (carboxycarbonyl)benzoic acid as a white solid. ESIMS calcd 195.0 (M+ + H), found 195.0 (M+ + H).

The synthetic route of Ethyl 2-(4-cyanophenyl)-2-oxoacetate has been constantly updated, and we look forward to future research findings.

Synthetic Route of 1897-52-5, The chemical industry reduces the impact on the environment during synthesis 1897-52-5, name is 2,6-Difluorobenzonitrile, I believe this compound will play a more active role in future production and life.

Take 2 L four bottles, add 600 mL of 60% sulfuric acid, electric stirring by adding 2,6_ difluorobenzonitrile 139.0 g (1.0 mol). Under N2 protection, the control reaction temperature was below 35 C, and 250 mum g of KBr03 (1.5 mol) was added to 10 batches. TLC monitoring, reaction 5-6 days, until the raw material point disappears, stop the reaction, the preparation of 800 mL 20% ice salt solution, the reaction solution Into the ice salt. After the product settling, the rapid filtration, the orange crude products, with CC14 dissolved crude products, respectively, with 5% Of NaHS03 solution, saturated Na2C03 solution and water to the solution was neutral, dried over anhydrous sodium sulfate, the solution was filtered, the water bath 60 C steamed to obtain light yellow liquid, rest for some time to cool into a pale yellow solid, vacuum distillation, warm water condensing steam, oil The bath was heated to 90 C and the fraction at a steam temperature of 58-62 C was cooled to give a white solid product in 71% yield

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, 2,6-Difluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Electric Literature of 1813-33-8, These common heterocyclic compound, 1813-33-8, name is 2-Chloro-4-(trifluoromethyl)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.

General procedure: Appropriate ROH (3.00 mmol) was added topotassium tert-butoxide (3.00 mmol) solution in toluene (7 ml).1,3-Dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone (DMPU, 3ml)was added to the mixture and stirred for 30 min at 80 C. Aftercooled down to ambient temperature of the reaction mixture,2-chloro-4-(trifluoromethyl)-benzonitrile (1.00 mmol) in toluenewas dropwise and stirred for 3 h at 80 C. The reaction wasquenched by adding water and extracted with EtOAc twice. Thecombined organic extracts were dried over MgSO4, filtered, andconcentrated in vacuo. The residue was purified by flash columnchromatography on silica gel using EtOAc/hexane (1:7) eluantcondition.

The synthetic route of 1813-33-8 has been constantly updated, and we look forward to future research findings.

Application of 53312-81-5, The chemical industry reduces the impact on the environment during synthesis 53312-81-5, name is 5-Amino-2-fluorobenzonitrile, I believe this compound will play a more active role in future production and life.

AM-1 -1 CN AM-1-1 amine To a solution of AM-1 -1_CN (1.36 g, 10 mmol) in MeOH (50 mL) was added CoCI2.6H20 (4.7 g, 20 mmol). NaBH4 (1.13 g, 30 mmol) was added in portions to the above mixture at 0 C. The reaction mixture was warmed to r.t. and continued stirring for 12 hrs. The reaction mixture was made pH=13 with NH3.H20 and extracted with EA. The combined organic layer was washed with brine, dried over Na2S04 and concentrated. The crude was purified by column chromatography on silica gel (DCM / MeOH, 9:1 ) to give the product (0.6 g, 43%).

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, 5-Amino-2-fluorobenzonitrile, other downstream synthetic routes, hurry up and to see.

Electric Literature of 17626-40-3, 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. 17626-40-3, name is 3,4-Diaminobenzonitrile, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of commercial o-phenylendiamines 1, 4-12 (1 mmol), 1-(4-formylpheny)-1H-benzimidazole (3) (1 mmol), and Na2S2O5 (1 mmol) in DMF (3 mL) was heated at 110-120C for 3 h.14 The reaction mixture was cooled, poured into H2O, and the solid was filtered. The residue was purified by column chromatography using chloroform/methanol (100:10) as eluant.

The chemical industry reduces the impact on the environment during synthesis 3,4-Diaminobenzonitrile. I believe this compound will play a more active role in future production and life.

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. 70591-86-5, name is 3-Bromobenzoylacetonitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H6BrNO

General procedure: To a solution of catalyst 4 (0.01mmol), 3,5-(NO2)2C6H3CO2H (0.02mmol), and alpha,beta-unsaturated aldehyde 2 (0.10mmol) in toluene (1.0mL) was added alpha-cyanoketones 1 (0.15mmol) at 0C. The resulting solution was then stirred for 48h. After complete consumption of the aldehyde (as monitored by TLC), the reaction mixture was evaporated and then loaded onto silica gel (ethyl acetate/petroleumether=1:10 to 1:7) and the products 3a-n were obtained by column chromatography. The title compound was obtained according to the general procedure (85% yield) as a mixture of two diastereoisomers (major and minor). Yellow solid; [alpha]D30=+31.3 (c 1.60, CHCl3); mp=170-172C; 1H NMR (400MHz, CDCl3): delta 7.89 (s, 1H; minor), 7.87 (s, 1H; major), 7.79 (d, J=8Hz, 1H; both diastereoisomers), 7.59 (d, J=8Hz, 1H; both diastereoisomers), 7.41-7.37 (m, 2H; both diastereoisomers), 7.33-7.28 (m, 4H; both diastereoisomers), 5.66-5.63 (m, 1H; major), 5.60-5.56 (m, 1H; minor), 3.95 (dd, J=9.6, 6.4Hz, 1H; major), 3.90 (dd, J=10.0, 6.4Hz, 1H; minor), 3.57 (d, J=4Hz, 1H; major), 3.54 (d, J=7.2Hz, 1H; minor), 2.52-2.46 (m, 1H; minor), 2.30-2.24 (m, 1H; major), 2.09-2.03 (m, 1H, both diastereoisomers); 13C NMR (100MHz, DMSO-d6): delta 162.0, 142.2, 141.9, 136.2, 133.8, 131.1, 131.0, 129.2, 128.4, 128.1, 127.7, 127.6, 121.9, 119.6, 97.4, 93.3, 88.5, 36.6, 35.9ppm; (additional peaks are observed due to diastereoisomers). IR (KBr): nu 3386.4, 2207.0, 1607.8, 1591.1, 1559.7, 1473.7, 1148.5, 1100.6, 1073.6, 950.9, 861.8, 829.0, 791.0, 765.5cm-1; d.r.: trans/cis=3.79/1; ESI-MS (m/z): 354.1 (M-H)-; HRMS(ESI): calcd for ([C18H14NO2BrNa+]): 378.0100. Found: 378.0100; enantiomeric excess: 92%, determined by HPLC (Chiralcel OD-H column, hexane/ i-PrOH 80:20, flow rate 0.7mL/min; lambda=254nm, tmajor=18.5min, tminor=11.2min).

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.