A kind of synthesis technique of trans-menthyl-2,8-dien-1-ol
A synthetic process, a menthyl-based technology, applied in the field of synthetic process of trans-menthyl-2,8-dien-1-ol, can solve problems such as unseen
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Embodiment 1
[0040] A synthesis technique of trans-menthyl-2,8-dien-1-ol, which comprises the steps:
[0041] (1) To the mixed system of (+)-limonene 1.2Kg, purified water 4L and myristic acid 205g, add Humicolap.lipase 48g, then slowly pump 1.1L hydrogen peroxide with a concentration of 30% at 23°C, control The pumping time was 16 hours. After the pumping, the reaction was continued for 2 hours to stop the reaction. The sodium sulfite aqueous solution with a concentration of 16.7% was added to quench, extracted with methyl tert-butyl ether, and the liquid was separated twice. Aqueous sodium bicarbonate solution and washing with water, and finally the organic phase after washing was distilled under reduced pressure to obtain 761 g of trans-1,2-epoxylimonene (purity 91.4%, yield 57%; cis-1,2-epoxylimonene content 1.6 %).
[0042] (2) Under nitrogen protection, 843 g of diphenyl diselenide and 7.6 L of absolute ethanol were mixed, the temperature was lowered to 8 °C, 234 g of sodium borohyd...
Embodiment 2
[0047] A synthesis technique of trans-menthyl-2,8-dien-1-ol, the difference between it and embodiment 1 is:
[0048] (1) To the mixed system of (+)-limonene 1.2Kg, purified water 4L and myristic acid 205g, add Humicolap.lipase 600g, then slowly pump 1.1L hydrogen peroxide with a concentration of 30% at 23°C, control The pumping time was 16 hours. After the pumping, the reaction was continued for 2 hours to stop the reaction. The sodium sulfite aqueous solution with a concentration of 16.7% was added to quench, extracted with methyl tert-butyl ether, and the liquid was separated twice. Aqueous sodium bicarbonate solution and washing with water, and finally the organic phase after washing was distilled under reduced pressure to obtain 745 g of trans-1,2-epoxylimonene (purity 90.1%, yield 56%; cis-1,2-epoxylimonene 1.8% );
[0049] (3) 501 g of trans-menthyl-2,8-dien-1-ol (purity 95.0%, ee% 99.0%,
[0050] de% 99.1%).
[0051] The overall yield of the reaction from compound 2 ...
Embodiment 3
[0054] A synthesis technique of trans-menthyl-2,8-dien-1-ol, the difference between it and embodiment 1 is:
[0055] (1) To the mixed system of (+)-limonene 1.2Kg, purified water 4L and myristic acid 205g, add Humicolap.lipase 48g, then slowly pump 2.2L hydrogen peroxide with a concentration of 30% at 23°C, control The pumping time was 24 hours. After the pumping, the reaction was continued for 2 hours to stop the reaction. The sodium sulfite aqueous solution with a concentration of 16.7% was added to quench, extracted with methyl tert-butyl ether, and the liquid was separated twice. Aqueous sodium bicarbonate solution and washing with water, and finally the washed organic phase was distilled under reduced pressure to obtain 776 g of trans-1,2-epoxylimonene (purity 89.2%, yield 54%; cis-1,2-epoxylimonene 2.3% );
[0056] (3) 516 g of trans-menthyl-2,8-dien-1-ol was finally obtained (purity 97.0%, ee% 98.4%, de% 98.9%).
[0057] The overall yield of the reaction from compound...
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