Reference of 2469-99-0, 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. 2469-99-0 name is 3-Oxobutanenitrile, 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.
Step 1. 2-(2-Chlorobenzyl)-3-oxobutanenitrile Into a 250-mL 3-necked round-bottom flask, was placed ethanol (100 mL). This was followed by the addition of Na (1.72 g, 74.78 mmol, 1.50 equiv) in several batches. The reaction was refluxed until the Na dissolved. To this was added a solution of 3-oxobutanenitrile (4.15 g, 50.00 mmol, 1.00 equiv) in ethanol (20 mL) dropwise with stirring, while the temperature was maintained at reflux. The reaction was refluxed for 1 h. Then, a solution of 1-(bromomethyl)-2-chlorobenzene (10.25 g, 50.00 mmol, 1.00 equiv) in ethanol (20 mL) was added dropwise with stirring, while the temperature was maintained at reflux. Refluxing continued for 2 hrs. Then the reaction was cooled to room temperature, concentrated to dryness and then suspended between water and ether. The aqueous layer was separated and extracted with ether. The aqueous layer was acidified with 3N HCl to pH<6 and extracted with EA. The organic layer was dried over Na2SO4, filtered and concentrated to dryness. The residue was chromatographed (PE:EA=1:50) to get 2.9 g (27%) of 2-(2-chlorobenzyl)-3-oxobutanenitrile as a colorless oil.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 3-Oxobutanenitrile, and friends who are interested can also refer to it.
Reference:
Patent; BIOENERGENIX; US2012/277224; (2012); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts