A kind of method that takes caprolactam as raw material to synthesize hexamethylene diamine
A technology of caprolactam and hexamethylene diamine, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc. Equipment requirements are easy, post-processing is convenient, and the reaction conditions are mild.
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Embodiment 1
[0031] A method for synthesizing hexamethylene diamine with caprolactam as a raw material, comprising the following steps:
[0032] 1) Add 10g of caprolactam into a 250ml single-neck bottle, add 11g of sodium hydroxide and 25ml of water, reflux at 130°C for 3 hours and then cool to room temperature to obtain 6-aminocaproic sodium salt; the molar ratio of the caprolactam to sodium hydroxide is about is 1:3; the molar ratio of caprolactam to the amount of water added is 1:15.8;
[0033] 2) then add 9ml acetic anhydride (amino protecting group, the amount of amino protecting group is 1 times of caprolactam equivalent) in the single-necked bottle of step 1), then to 47 ℃, add concentrated hydrochloric acid after stirring reaction for 2 hours to adjust The pH value of the solution is at 2, and the precipitated solid is recrystallized with water to obtain 6-acetamidocaproic acid;
[0034] 3) drying the product of step 2) to obtain 12g solid; get the product after drying 5g and 0.15...
Embodiment 2
[0037] A method for synthesizing hexamethylene diamine with caprolactam as a raw material, comprising the following steps:
[0038] 1) Add 10g of caprolactam into a 250ml single-neck bottle, and add 13g of sodium tert-butoxide and 32ml of water, reflux at 150° C. for 2 hours and then cool to room temperature to obtain 6-aminocaproic sodium salt; the moles of caprolactam and sodium tert-butoxide are obtained. The ratio is about 1:1.5; the molar ratio of caprolactam to the amount of added water is 1:20;
[0039]2) Then slowly add 18ml benzyl chloroformate (the amino protecting group, the amount of the amino protecting group is 1.5 times the caprolactam equivalent) into the single-necked bottle of step 1), and add to the reaction solution after stirring for 2 h at room temperature. 30ml diethyl ether was used to extract the by-products in the reaction, repeat the operation twice, then add concentrated hydrochloric acid to the extracted aqueous layer solution under ice bath to adj...
Embodiment 3
[0043] A method for synthesizing hexamethylene diamine with caprolactam as a raw material, comprising the following steps:
[0044] 1) Add 10g of caprolactam into a 250ml single-neck bottle, add 7g of sodium hydroxide and 16ml of water, reflux at 100°C for 4h and then cool to room temperature to obtain 6-aminocaproic sodium salt; the molar ratio of the caprolactam to sodium hydroxide is about is 1:2; the molar ratio of caprolactam to the amount of water added is 1:10;
[0045] 2) Then slowly add 15ml of tetrahydrofuran and 20ml of benzyl chloride (the amino protecting group, the amount of the amino protecting group is 2 times the equivalent of caprolactam) into the single-necked bottle of step 1), react under reflux at 70°C for 10h, and cool to room temperature , and concentrated hydrochloric acid was added to the obtained solution to adjust the pH value of the solution to 3; after the reaction, 20 ml of ethyl acetate was added to extract the product, and the operation was rep...
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