N-acyl-1,2-ring nitrogen p-menthane and its preparation method and application of herbicidal activity
A ring nitrogen p-menthane and acyl technology, which is applied in the field of N-acyl-1,2-ring nitrogen p-menthane and its preparation, can solve the problems of inapplicability and non-discovery, and achieve low environmental pollution, low toxicity, The effect of strong herbicidal activity
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Embodiment 1
[0046] Add 19.9 mL of 10% HCl aqueous solution, 5.08 g of N,N'-acyl-1,8-p-mentanediamine (such as N, N'-Diacetyl-1,8-p-mentanediamine, N,N'-dibutyryl-1,8-p-mentanediamine, N,N'-dipentanoyl-1,8-p Menthanediamine, N,N'-dicaproyl-1,8-p-mentanediamine, N,N'-dibenzoyl-1,8-p-menthanediamine and N,N'-di Phenylacetyl-1,8-p-menthanediamine, etc.), heated to reflux for 26h. After the reaction was completed, it was left to stand, and the reaction solution was separated into layers. After the pH of the lower layer solution was adjusted to 8-11, the solution was layered, and the upper layer solution was dried and subjected to silica gel column chromatography to obtain the corresponding N-acyl-1,2-cycloaza-p-menthane product.
Embodiment 2
[0048] In the 100mL four-neck flask equipped with a thermometer, a condenser tube and a mechanical stirrer, add 20mL concentration of 10% HCl aqueous solution, 2g N-acyl-3-p-mentene-1-amine (such as N-acetyl-3- p-menten-1-amine, N-butyryl-3-p-menten-1-amine, N-pentanoyl-3-p-menten-1-amine, N-hexanoyl-3-p-menten-1 -amine, N-benzoyl-3-p-menthene-1-amine and N-phenylacetyl-3-p-menthen-1-amine, etc.), heated to reflux for 24h. After the reaction was completed, it was left to stand, and the reaction solution was separated into layers. After the pH of the lower layer solution was adjusted to 8-11, the solution was layered, and the upper layer solution was dried and subjected to silica gel column chromatography to obtain the corresponding N-acyl-1,2-cycloaza-p-menthane product.
Embodiment 3
[0050] Add 198.9mL of 10wt.% HCl aqueous solution and 50.8g of N,N'-diacetyl-1,8-p-mentanediamine to a 500mL four-necked flask equipped with a thermometer, a condenser and a mechanical stirrer, Start stirring, heating to reflux for 30h. After the reaction, it was left standing, and the reaction solution was separated into layers, the upper layer was a yellow liquid, and the lower layer was an aqueous solution. After the pH of the lower layer solution was adjusted to 8-11, the solution was layered, and the upper layer was a yellow transparent liquid. The yellow transparent liquid in the upper layer was vacuum-dried at 70° C. to obtain 11.8 g of the product, with a yield of 30.3%. After silica gel column chromatography, a colorless and transparent liquid product with a purity of 99.85% was obtained, and its main physical parameters and HR-MS, FT-IR, ESI + -MS, 1 H-NMR and 13 C-NMR characterization data are as follows:
[0051] Boiling point B.p.=229.3°C; Refractive index ...
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