A kind of n-dodecyl ethyl imidate methyl ester and its synthetic method
A technique for the synthesis of methyl dodecyl acetimidate and its synthesis method, which is applied in the field of organic synthesis and synthesis, can solve the problems of complex reaction process, no public literature report on the production method, and low yield of imidate, and achieve The production process is simple, fills the blank of production technology, and has the effect of high yield
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Embodiment 1
[0036] This embodiment provides a kind of N-dodecyl acetimidic acid methyl ester, which is synthesized through the following steps:
[0037] Weigh 1.89 g of dodecylamine into a four-necked flask with a condenser, vacuum device and thermometer, add 20 mL of methanol, and heat in a constant temperature oil bath until dodecylamine is completely dissolved;
[0038] When the temperature rises to 70°C, slowly drop 1.70g of N,N-dimethylacetamide dimethyl acetal into the solution, and react at 0.1MPa for 180min;
[0039] TLC (V CHCl3:CH3OH =3:1) sample climbing board, no raw material point occurs, indicating that dodecylamine is fully converted;
[0040] Reduce the pressure to 0.01MPa, and continue the reaction at 60°C for 30 minutes to obtain a light yellow liquid product, which is methyl N-dodecylethyleneimidate, the yield of methyl N-dodecylethyleneimidate was 71.4%.
[0041] The mass spectrogram (diluted in acetonitrile) of the product synthesized in this embodiment is as follo...
Embodiment 2
[0046] This embodiment provides a kind of N-dodecyl acetimidic acid methyl ester, which is synthesized through the following steps:
[0047] Weigh 1.92g of dodecylamine into a four-necked flask with a condenser, vacuum device and thermometer, add 30mL of methanol, and heat in a constant temperature oil bath until dodecylamine is completely dissolved;
[0048] When the temperature rises to 40°C, slowly drop 1.60g of N,N-dimethylacetamide dimethyl acetal into the solution, and react for 10h at 0.1MPa;
[0049] TLC (V CHCl3:CH3OH =3:1) sample climbing board, no raw material point occurs, indicating that dodecylamine is fully converted;
[0050] Reduce the pressure to 0.03MPa, continue the reaction at 50°C for 1h, and obtain a light yellow liquid product, which is methyl N-dodecylethylimidate. The yield of ester was 72.2%.
[0051] The above examples illustrate that in the synthetic method of N-dodecylethylimidate methyl ester of the present invention, the yield of N-substitute...
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