Preparation of 2-methylbenzophenone_Kain Industrial Additive

Background and overview^[1]

2-Methylbenzophenone is a benzophenone compound and a very important fine chemical. At the same time, ketones are also the core structure of many organic molecules, such as functional materials, spices and drug molecules. Aromatic ketones are very important synthetic building blocks in organic synthesis. They are widely present in the core structures of natural products and are widely used in biologically active compounds.

Preparation^[1]

CN201810156179.8 reports a preparation method of aromatic ketones. The raw materials used in the preparation method are cheap and easy to obtain, have good stability, and the reaction conditions are mild. The method is that under the action of a palladium catalyst and a nitrogen-containing ligand, a nitrile compound reacts with an arylsulfonyl hydrazide in an organic solvent, and after the reaction is completed, the aromatic ketone is obtained through post-treatment. (1) The raw materials used in this method are cheap and easy to obtain, have good stability, and the reaction conditions are mild. (2) This method is not only applicable to aromatic nitrile compounds, but also to aliphatic nitrile compounds. The reaction has wide substrate applicability and functional group tolerance, and has potential application value in the construction of aryl-carbonyl groups. . The specific operations are as follows:

Under inert gas protection, 2-methylphenylsulfonylhydrazide (1.1mmol), benzonitrile (1.0mmol), palladium catalyst (2mol%) and biquinoline (bq, 3mol%) were dispersed in an organic into the solvent (2 mL), then add H₂O (2 mmol), raise the temperature to 80°C and react for 6 hours. Then the reaction solution was extracted three times with Et₂O (5mL), the organic phases were combined, and the solvent was spin-dried under reduced pressure. The obtained crude product was subjected to column chromatography on a silica gel column (300-400 mesh), and the The removing agent is a mixture of petroleum ether and ethyl acetate to obtain the target product 2-methylbenzophenone.