N-acetyl-3-foxlene-1-amine and preparation method thereof
A technology for p-menene and acetyl group, which is applied in the field of synthesis of N-acetyl-3-p-menene-1-amine, can solve the problems of difficulty in product separation and purification, and achieves good prospects for industrial application and controllable environmental pollution. , the effect of less environmental pollution
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Embodiment 1
[0040] Add 369mL of 7.5% HCl aqueous solution and 101.6g (400mmol) of N,N'-diacetyl-1,8-p-menthanediamine to a 1L four-neck flask equipped with a thermometer, condenser and mechanical stirrer , Start stirring, and heat to reflux for 6h. After the reaction was finished, the reaction liquid was cooled, and the layers were separated. The yellow oily liquid in the upper layer was evaporated in vacuo to obtain 43.0 g of crude product (yellow oily viscous substance) with a content of 78%. The crude product was separated and purified by silica gel column chromatography to obtain 21.0 g (107.7 mmol) of N-acetyl-3-p-menten-1-amine product with a purity of 92%, and a yield of 26.9%.
Embodiment 2
[0042] Weigh 50g of silica gel with a specification of 200-300 mesh into a 100mL beaker, add an appropriate amount of petroleum ether (60-90°C), stir it into a paste, and pour it into a chromatography column with a sand core. Weigh 2 g of crude N-acetyl-3-p-menten-1-amine obtained in Example 1 with a content of 78%, dissolve it with a small amount of eluent, and load it. When the liquid level of the chromatographic column is about to disappear, add an appropriate amount of quartz sand, and add an eluent for eluting, and the eluent is ethyl acetate petroleum ether solution (V 乙酸乙酯 :V 60-90℃石油醚 =3︰8)), use a 10mL test tube to receive the eluate, and use gas chromatography to analyze the eluate in each test tube, and combine the high-purity N-acetyl-3-p-mentene-1-amine The eluate was concentrated and dried in vacuo to obtain 1.48 g of light yellow viscous solid product with a purity of 95% N-acetyl-3-p-menten-1-amine. FT-IR, ESI + -MS, 1 HNMR and 13 The characterization data...
Embodiment 3
[0045] Add 19.9mL of 10% HCl aqueous solution, 5.08g of N,N'-diacetyl-1,8-p-menthanediamine (20mmol ), heated to reflux for 6h. After the reaction, the reaction liquid was cooled, and the reaction liquid was analyzed by gas chromatography. The results showed that the yield of N-acetyl-3-p-menten-1-amine was 48.2%. And according to the separation method of Example 1 and Example 2, the above reaction solution was processed to obtain 1.31 g of N-acetyl-3-p-menthen-1-amine product.
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