α-(n-benzyl)amino-ε-caprolactam compound and its preparation method and application
A technology of caprolactam and compounds, which is applied in the field of α-(N-benzyl)amino-ε-caprolactam compounds and their preparation, can solve problems such as reports of successful research and development that have not yet been found, and achieve the effect of improving strength and heat resistance
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Embodiment 1
[0031] Example 1: Preparation of α-(N-(2-hydroxybenzyl))amino-ε-caprolactam.
[0032]
[0033] Add 16.5 g (0.1 mol) of α-amino-ε-caprolactam hydrochloride, 10.6 g (0.1 mol) of sodium carbonate and 500 ml of methanol into a 1-L three-necked flask, and stir to dissolve. At room temperature, 18.3 g (0.15 mol) of 2-hydroxybenzaldehyde was added, and the reaction was continued for 1 hour with stirring. The reaction solution was transferred to the condition of 0°C, and 4.54 g (0.12 mol) of sodium borohydride as a reducing agent was added and reacted for 1 hour. After the reaction, methanol was removed by distillation under reduced pressure, dissolved by adding 500ml of dichloromethane, washed with 100ml of distilled water 3 times, washed with saturated brine once, dried with anhydrous sodium sulfate, filtered, collected the filtrate, and distilled under reduced pressure to obtain the result Crude. The crude product was recrystallized with ether to obtain 18.5 g of α-(N-(2-hydroxybenz...
Embodiment 2
[0034] Example 2: Preparation of α-(N-(2-chlorobenzyl))amino-ε-caprolactam.
[0035]
[0036] Add 16.5 g (0.1 mol) of α-amino-ε-caprolactam hydrochloride, 10.6 g (0.1 mol) of sodium carbonate and 500 ml of methanol into a 1-L three-necked flask, and stir to dissolve. Under the condition of 30°C, 16.9 g (0.12 mol) of 2-chlorobenzaldehyde was added, and the stirring was continued for 0.5 hour. The reaction solution was transferred to a condition of 5°C, and 3.78 g (0.10 mol) of sodium borohydride as a reducing agent was added and reacted for 4 hours. After the reaction, methanol was removed by distillation under reduced pressure, dissolved by adding 500ml of dichloromethane, washed with 100ml of distilled water 3 times, washed with saturated brine once, dried with anhydrous sodium sulfate, filtered, collected the filtrate, and distilled under reduced pressure to obtain the result Crude. The crude product was recrystallized with ether to obtain 16.18 g of α-(N-(2-chlorobenzyl))ami...
Embodiment 3
[0037] Example 3: Preparation of α-(N-(3-methylbenzyl))amino-ε-caprolactam.
[0038]
[0039] Add 16.5 g (0.1 mol) of α-amino-ε-caprolactam hydrochloride, 4.0 g (0.1 mol) of sodium hydroxide and 500 ml of methanol into a 1-L three-necked flask, and stir to dissolve. Under the condition of 30°C, 21.6 g (0.18 mol) of 3-methylbenzaldehyde was added, and the reaction was continued to be stirred for 4 hours. The reaction solution was transferred to -5°C, and 7.54 g (0.12 mol) of sodium cyanoborohydride as a reducing agent was added and reacted for 8 hours. After the reaction, methanol was removed by distillation under reduced pressure, dissolved by adding 500ml of dichloromethane, washed with 100ml of distilled water 3 times, washed with saturated brine once, dried with anhydrous sodium sulfate, filtered, collected the filtrate, and distilled under reduced pressure to obtain the result Crude. The crude product was recrystallized with ether to obtain 15.47 g of α-(N-(3-methylbenzyl))...
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