Category: 110301-23-0

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. 110301-23-0, name is 4-Amino-3,5-difluorobenzonitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H4F2N2

The benzaldehyde used as starting material was prepared as follows; To a stirred solution of 4-amino-3,5-difluorobenzonitrile (2.Og, 12.98mmol) in toluene (16ml) was added dropwise DIBAL (1.5M in toluene) at O0C. The reaction mixture was warmed to RT and stirring continued for 2h. The reaction was quenched by dropwise addition to 10% aq citric acid (10ml). EtOAc (50ml) and saturated aq potassium sodium tartrate (Rochelle’s salt) (30ml) were added and the mixture was vigorously stirred for 20min. The organic layer was isolated and washed with water (10ml), dried (Na2SO4), filtered and concentrated to dryness to give a pale yellow solid (1.9g, 93%). LCMS purity 92%, m/z 158 [M+H]+.

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.

Reference:
Patent; CHROMA THERAPEUTICS LTD.; WO2007/129040; (2007); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 110301-23-0, name is 4-Amino-3,5-difluorobenzonitrile, A new synthetic method of this compound is introduced below., Formula: C7H4F2N2

Step 4 4 g of sodium nitride was added to 30 ml of concentrated sulfuric acid and chilled to a temperature of 10 C. and 38 ml of acetic acid was added thereto. 8.9 ml of 4-cyano-2,6-difluoroaniline was added gradually to maintain the solution at a temperature of 20 to 25 C. The reaction mixture was added dropwise to a solution a 10 g of copper (I) bromide dissolved in 30 ml of concentrated hydrobromic acid. After the dropwise addition was completed, the reaction mixture was stirred for one and one half hours at room temperature. Water was added to the reaction mixture, the reaction mixture was extracted with chloroform and washed with water. The organic layer was removed by distillation, and the residue was recrystallized with a mixture of methanol and acetone to yield 6.6 g of 2-bromo-5-cyano-1,3-difluorobenzene.

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.

Reference:
Patent; Seiko Epson Corporation; US4883609; (1989); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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 110301-23-0 as follows. HPLC of Formula: C7H4F2N2

Step 9 While stirring 420 cm3 of concentrated sulfuric acid on an ice water bath, 54 g (0.78 mol) of finely pulverized NaNO2 was added at a rate which maintained the temperature below 40 C. The mixture was stirred on a warm water bath at 50 C. until the crystals were completely dissolved. The solution was stirred on an ice water bath and 700 cm3 of glacial acetic acid was added drop-wise. 108 g (0.70 mol) of 4-amino-3,5-difluorobenzonitrile was added at a rate which maintained the temperature at 20-25 C. and the mixture was stirred at that temperature until the crystals were completely dissolved to form the corresponding diazonium salt. An aqueous solution of the diazonium salt was added drop-wise for 2 hours to a solution of 143 g (1.0 mol) of copper (I) bromide dissolved in 420 cm3 of 47% hydrobromic acid while stirring on an ice water bath. The resulting solution was stirred for one hour on an ice water bath and allowed to sit overnight at room temperature. The product was filtered, washed with glacial acetic acid and recrystallized from a solvent mixture of acetone and methanol to yield 98 g (0.45 mol) of 4-bromo-3,5-difluorobenzonitrile.

According to the analysis of related databases, 110301-23-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Seiko Epson Corporation; US5200110; (1993); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts