Preparation method of herbac spice
An Averman ketone fragrance and reaction technology, which is applied in the directions of essential oils/fragrance, oxidative preparation of carbonyl compounds, organic chemistry, etc., can solve problems such as high cost, and achieve the effects of reducing production cost and high yield
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Embodiment 1
[0025] Under nitrogen protection, a copper-chromium catalyst (Cu 2 Cr 2 o 5 ) powder (6.0 g, BASF CORPORATION, CAMPUS DRIVE FLORHAM PARK, NJ07932USA, model: Cu O2O2P) and paraffin oil (primol, 20 g). Under mechanical stirring, the temperature was raised to 210°C. Through the dropping funnel, 300 grams of the alicyclic alcohol intermediate (the alicyclic alcohol intermediate is a mixture of the compound of formula (a) and the compound of formula (b), purchased from International Perfume and Fragrance Company, CP alcohol) was added dropwise in one hour. After the dropwise addition, the reaction reflux temperature was maintained until the conversion of the starting material was figure 1 ). GC-MS results showed that M=154.1 of formula (I) and M=154.2 (molecular weight=154.14) of formula (I), confirming that the desired avermanone fragrance product was obtained.
[0026] The distillation residue and catalyst were reused for the reaction, and the reaction activity was not observ...
Embodiment 2
[0030] Under nitrogen protection, a copper-zinc-aluminum catalyst (Cu-ZnO-Al 2 o 3 ) powder (5.0 g, Shanghai Xunkai New Material Technology Co., Ltd., model: loaded copper Cu-1000T) and paraffin oil (primol, 50 g). Under mechanical stirring, the temperature was raised to 210°C. Through the dropping funnel, 250 grams of the alicyclic alcohol intermediate (purchased from International Perfume and Fragrance Company, CP alcohol) was added dropwise for one hour. After the dropwise addition, the reaction reflux temperature was maintained until the conversion of the starting material was detected by GC to <2% (GC%, about 10 hours). After cooling down to room temperature, the crude product solution was distilled by vacuum distillation under oil pump vacuum, and further obtained 240 g of colorless liquid (93% molar yield) by rectification column vacuum distillation. The product was analyzed by GC-MS, which confirmed that the desired avermanone fragrance product was obtained.
Embodiment 3
[0032]Under nitrogen protection, add copper-zinc catalyst (CuO-ZnO-promoter) grinding powder (8.0 g, Liaoning Haitai Science and Technology Development Co., Ltd. , model: CHDH-1) and paraffin oil (primol, 50 g). Under mechanical stirring, the temperature was raised to 210°C. Through the dropping funnel, 300 grams of the alicyclic alcohol intermediate (purchased from International Fragrance and Fragrance Company, CP alcohol) was added dropwise for one hour. After the dropwise addition was complete, the reaction reflux temperature was maintained until the conversion of the starting material was detected by GC to <2% (GC%, about 8 hours). After cooling down to room temperature, the crude product solution was distilled off by rectification under reduced pressure in an oil pump vacuum, and then further rectified under reduced pressure using a rectifying column to obtain 279 grams (93% molar yield). The product was analyzed by GC-MS, which confirmed that the desired avermanone fra...
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