Introduction of a new synthetic route 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.

Adding a certain compound to certain chemical reactions, such as: 26391-06-0, name is 2-Cyano-N,N-diethylacetamide, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 26391-06-0, Recommanded Product: 2-Cyano-N,N-diethylacetamide

Example 1; Mixture of the E and Z isomers of N,N-diethyl-2-cvano-3-(3,4-dihydroxy-5- nitrophenvDacrylamide[0031 ] A vessel is charged with 240 ml of n-butanol, 120 g of 3,4-dihydroxy-5- nitrobenzaldehyde, 4.8 g of methylamine hydrochloride, 122 g of N5N- diethylcyanoacetamide and 7.2 ml of piperidine. The temperature is raised using water separation under vacuum to about 82 0C and the reaction mixture is boiled at this temperature using water separation for 4 hours. The reaction is followed using HPLC.[0032] After completing the reaction 240 ml of hot water is added to the reaction mixture and 2.4 ml of strong sulphuric acid is added.[0033] The reaction mixture is cooled to a temperature of 75 C and seeded with crude N,N-diethyl-2-cyano-3-(3,4-dihydroxy-5-nitrophenyl)acrylamide (comprises 70 % by weight of the E- isomer). After seeding the mixture is cooled to about 28 C within 3 hours, during which time the E isomer crystallizes.[0034] The reaction mixture is seeded with a mixture of the E and Z isomers of N9N- diethyl-2-cyano-3-(3,4-dihydroxy-5-nitrophenyl)acrylamide (comprises about 30 % by weight of the Z- isomer) and mixed at about 28 C for two hours. Thereafter the mixture is cooled slowly to 0 0C during which time the Z isomer crystallizes.[0035] The mixture is filtered and washed twice with 60 ml of cold water and the filtering cake is dried. The yield is about 90 % and the purity over 99.5 %.Example 2 Mixture of the E and Z isomers of N,N-diethyl-2-cvano-3-(3,4-dihvdroxy-5- nitrophenvDacrylamide[0036] A vessel is charged with 180 ml of n-butanol, 120 g of 3,4-dihydroxy-5- nitrobenzaldehyde, 2.9 g of methylamine hydrochloride, HO g of N9N- diethylcyanoacetamide and 4.3 ml of piperidine. The temperature is raised using water separation under vacuum to about 82 0C and the reaction mixture is boiled at this temperature using water separation for 5 hours. The reaction is followed using HPLC.[0037] After completing the reaction 180 ml of hot water is added to the reaction mixture and 12 ml of strong sulphuric acid is added.[0038] The reaction mixture is cooled to a temperature of 75 0C and seeded with crude N,N-diethyl-2-cyano-3-(3,4-dihydroxy-5-nitrophenyl)acrylamide (comprises 70 % by weight of the E- isomer). After seeding the mixture is cooled to about 28 0C within 2 hours, during which time the E isomer crystallizes.[0039] The reaction mixture is seeded with a mixture of the E and Z isomers of N5N- diethyl-2-cyano-3-(3,4-dihydroxy-5-m’trophenyl)acrylamide (comprises about 30 % by weight of the Z- isomer) and mixed at about 28 C for two hours. Thereafter the mixture is cooled slowly to 0 0C during which time the Z isomer crystallizes.[0040] The mixture is filtered and washed twice with 100 ml of cold water and the filtering cake is dried. The yield is about 96% and the purity over 99.5 %.

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; ORION CORPORATION; WO2007/90923; (2007); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts