Maleimide type compound, as well as preparation and application thereof
A technology of maleimide and maleic anhydride is applied in the field of antibacterial agent and preparation and application, and can solve problems such as affecting product quality, economic loss and the like
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example 1
[0043] Example 1: N-n-butyl-maleimide (I-1)
[0044] Weigh 1.47g (0.015mol) of maleic anhydride into a dry three-neck flask equipped with a magnetic stirrer, add 10mL of glacial acetic acid to dissolve, measure 1.10g (0.015mol) of n-butylamine, and dissolve it with 10mL of glacial acetic acid, Add it to the constant pressure funnel drop by drop, stir while adding, after 20 minutes to complete the dropwise addition, heat to 70-80°C, react for 3h, after the reaction is completed, cool the reaction solution to room temperature, distill under reduced pressure, and remove the solvent , to obtain a concentrated solution, the concentrated solution was subjected to silica gel column chromatography (eluent V 石油醚 :V 乙酸乙酯 =5:1), the target liquid was collected and concentrated to obtain 1.75 g of a yellow oily liquid product with a yield of 75.1% (based on the mass of maleic anhydride, the same below). The resulting product was 1 H NMR and MS spectroscopic analysis confirmed that it w...
Embodiment 2
[0047] Example 2: N-n-pentyl-maleimide (I-2)
[0048]Weigh 1.47g (0.015mol) of maleic anhydride into a dry three-neck flask equipped with a magnetic stirrer, and dissolve it in 15mL of benzene, measure 1.305g (0.015mol) of n-pentylamine, dissolve it in 15mL of benzene, and add Add drop by drop in the constant pressure funnel, stirring while dropping, about 10min after the dropwise addition is completed, the temperature rises to 115°C for reflux reaction for 3h; The concentrated solution was separated by silica gel column chromatography (eluent V 石油醚 :V 乙酸乙酯 =6:1), the target solution was collected and concentrated to obtain 1.81 g of a light yellow liquid product with a yield of 72.2%. The resulting product was 1 H NMR and MS spectroscopic analysis confirmed that it was N-n-pentyl-maleimide (I-2).
[0049] 1 H NMR (500MHz, CDCl 3 )δ6.71(s,2H),3.64–3.57(m,2H),1.63(dt,J=14.9,7.5Hz,2H),1.40–1.24(m,4H),0.91(t,J=7.2Hz ,3H).EIMS m / z(%):167.1(49)[M] + ,138.1(8),124.1(15),110....
Embodiment 3
[0051] Example 3: N-n-hexyl-maleimide (I-3)
[0052] Change the organic amine in Example 1 to 1.515g (0.015mol) n-hexylamine, and the other reaction operations are the same as in Example 1. After the dropwise addition is completed, heat at 120°C for reflux reaction for 3h. After the reaction is completed, the reaction solution is cooled to room temperature. Continuously add sodium bicarbonate aqueous solution with a mass concentration of 5% into the reaction solution, stir and shake until no bubbles are generated, separate the liquids to obtain the organic phase, distill under reduced pressure to obtain a concentrated solution, and carry out silica gel column chromatography on the concentrated solution Separation (eluent V 石油醚 :V 乙酸乙酯 =5:1), the target liquid was collected and concentrated to obtain 1.90 g of oily product with a yield of 70.1%. The resulting product was 1 H NMR and MS spectroscopic analysis confirmed that it was N-n-hexyl-maleimide (I-3).
[0053] 1 H NMR...
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