Category: 251570-03-3

Reference of 251570-03-3, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 251570-03-3 name is 2-(4-Chloro-3-fluorophenyl)acetonitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A mixture of the product of example 22 (7.8g, 0.046 mol), water (7.5 ml), concentrated sulfuric acid (7.5ml) and acetic acid (7.5ml) was heated at reflux for 2 hours . After being cooled to room temperature, the mixture was poured into ice-water. The resulting solids were collected by filtration and washed by diethyl ether to give the titled product (6.8g, 79%)1H NMR (300 MHz, DMSO-/) 3.64 (s, 2H), 7.14 (ddd, J= 0.6, 2.1, 8.2 Hz, IH), 7.34 (dd, J= 2.1, 10.6 Hz, IH), 7.52 (t, J=8.1 Hz, IH).MS (ESI”) m/z 187 (M-I)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(4-Chloro-3-fluorophenyl)acetonitrile, and friends who are interested can also refer to it.

Reference:
Patent; AVEXA LIMITED; DEADMAN, John, Joseph; JONES, Eric, Dale; LE, Giang, Thanh; RHODES, David, Ian; THIENTHONG, Neeranat; VAN DE GRAFF, Nicholas, Andrew; WINFIELD, Lisa, Jane; WO2010/31; (2010); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Synthetic Route of 251570-03-3, 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 251570-03-3 as follows.

2 -(4-Chloro-3-fluorophenyl)-2-methylpropanenitrileA solution of 4-chloro-3-fluorophenylacetonitrile (1.70 g, 10.0 mmol) in DMF (5 mL) was added dropwise to Sodium hydride (1.00 g, 41.7 mmol) and iodomethane (1.87 mL, 30.0 mmol) in DMF (10 mL) at O0C under a blanket of argon. The resulting slurry was stirred and allowed to warm to ambient temperature for 2 hours. The mixture was concentrated and diluted with ethyl acetate and water and the organic layer washed with further water and the organic layer washed with saturated brine, dried over MgSO4, filtered and evaporated. The crude product was purified by flash silica chromatography, elution gradient 0 to 5% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford 2-(4-chloro-3-(trifluoromethoxy)phenyl)-2-methylpropanenitrile as a yellow oil which solidified on standing.MS (+ve ESI) : Rt = 2.51 min, no mass ion (M+H)+ 1U NMR (400.132 MHz, CDC13) delta 1.71 (6H, s), 7.20 – 7.28 (3H, m), 7.42 (IH, t)

According to the analysis of related databases, 251570-03-3, the application of this compound in the production field has become more and more popular.