Month: April 2021

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.

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.