Continuously updated synthesis method about 2-Cyano-N,N-diethylacetamide

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Cyano-N,N-diethylacetamide, and friends who are interested can also refer to it.

Related Products of 26391-06-0, 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. 26391-06-0 name is 2-Cyano-N,N-diethylacetamide, 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.

1: Preparation of racemic 2-cvano-3-(3,4-dihvdroxy-5-nitrophenyl)-N,N-diethylprop-2~ en amide3,4-dihydroxy-5-nitro-benzaldehyde (5Og) and N,N-diethyl-2-cyano acetamide (99.4g) were taken together in dry ethanol (100OmL) and refluxed at 75-8O0C for 15-20min. followed by the addition of ammonium acetate (27g) lot-wise over a period of 24hrs at every 2 hours of interval. After completion of reaction the content was cooled to room temperature and the ethanol was distilled off under vacuum. The residue was taken in dichloromethane (100OmL) and stirred for 15min at 25-300C followed by the addition of purified water (100OmL) and stirred at 25-3O0C for 1 hr. The layer if not cleared was filtered through hyflobed and washed with methylene chloride. The organic layer was separated and the aqueous layer was washed with dichloromethane twice. The organic layer were combined and treated with dilute hydrochloric acid 30OmL (1:1 ratio of HCl and water). The organic layer was separated and treated with purified water to remove any undissolved impurities, the water treatment was repeated two to three times and further the organic layer was treated with activated carbon at 25-30 C and filtered. The filtrate distilled off under vacuum at 600C and the residue was taken in ethyl alcohol at 25-3O0C, stirred for 15- 20min. and distilled off under vacuum at 350C. To the residue was added purified water and the stirred for 2 hrs at 25-300C3 filtered and washed with water and dried to obtain racemic 2-cyano- 3-(3,4-dihydroxy-5-nitrophenyl)-N,N-diethylprop-2-enamide.(Dry Weight : 6Og (72.20%), HPLC purity : 98.32%, E isomer (69.80%) and Z isomer (28.52%)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-Cyano-N,N-diethylacetamide, and friends who are interested can also refer to it.

Reference:
Patent; NEULAND LABORATORIES LTD; WO2009/84031; (2009); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts