Preparation method of lyral and its application in cosmetic testing
A technology of new lilial and crude products, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve the problems of inconvenient use, expensive reference substances, and difficulty in obtaining them
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Embodiment 1
[0095] Add 539g (3.5mol) myrcenol and 0.539g hydroquinone to the 1000mL four-necked flask equipped with a thermometer, a mechanical stirring device and a reflux condenser, and heat to 110°C; add 235g ( 4.2mol) acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction flask was placed in a freezing tank, and the temperature of the reaction flask was kept at 110°C to 130°C; after the dropwise addition of acrolein, the reaction was continued for 1 hour to obtain the reaction mixture;
[0096] The reaction mixture was washed three times with 200 g of deionized water to obtain a crude product of 765 g of lily-aldehyde (the content of lily-aldehyde measured by GC was 94.74%); the crude product was rectified under a vacuum of 2 mmHg, and collected at a temperature of The fraction between 125°C yielded 612 g of lily-aldehyde (the content of lily-aldehyde measured by GC was 99.72%).
[0097] The obtained lily of the valley aldehyde fraction (about 1 / 4 of the ...
Embodiment 2
[0099]Add 539g (3.5mol) myrcenol and 0.539g hydroquinone to the 1000mL four-necked flask equipped with a thermometer, a mechanical stirring device and a reflux condenser, and heat to 110°C; add 216g ( 3.86mol) acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction flask was placed in a freezing tank, and the temperature of the reaction flask was kept at 110°C to 130°C; after the dropwise addition of acrolein, the reaction was continued for 1 hour to obtain the reaction mixture;
[0100] The reaction mixture was washed three times with 180 g of deionized water to obtain a crude product of 758 g of lilylaldehyde (the content of lilylaldehyde was 94.41% as measured by GC); The fraction between 125° C. yields 606 g of lily-aldehyde (the content of lily-aldehyde measured by GC is 99.69%).
[0101] The obtained lily of the valley aldehyde fraction (about 1 / 4 of the amount, multiplied by the remainder) is introduced into the potassium chloride powder tha...
Embodiment 3
[0103] Add 539g (3.5mol) myrcenol and 0.539g hydroquinone to the 1000mL four-necked flask equipped with a thermometer, a mechanical stirring device and a reflux condenser, and heat to 110°C; add 196g ( 3.5mol) acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction flask was placed in a freezing tank, and the temperature of the reaction flask was kept at 110°C to 130°C; after the dropwise addition of acrolein, the reaction was continued for 1 hour to obtain the reaction mixture;
[0104] The reaction mixture was washed three times with 180 g of deionized water to obtain a crude product of 748 g of lilylaldehyde (the content of lilylaldehyde was 88.46% by GC); The fraction between 125° C. yields 502 g of lily-aldehyde (the content of lily-aldehyde measured by GC is 99.41%).
[0105] The obtained lily of the valley aldehyde fraction (about 1 / 4 of the amount, multiplied by the remainder for use) is introduced into the potassium chloride powder that is...
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