Menthyl pyruvate cooling agent and preparation method thereof
A technology of menthyl pyruvate and menthyl lactate, applied in the field of physiological cooling agent menthyl pyruvate and preparation thereof, can solve the problems of strong cooling effect, high volatility and irritation, shortness and the like, and achieve lasting cooling effect, Improve heart function, excellent effect
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Embodiment 1
[0048] Add 300 ml of dichloromethane into a 1000 ml four-necked flask equipped with a stirring, thermometer, condenser and constant pressure dropping funnel, and add 500 g of menthyl lactate (2.2moL, 1eq), 28 g of sodium bromide ( 0.27moL, 0.12eq), after the menthyl lactate is completely dissolved, slowly add 300 ml of 27.5% hydrogen peroxide (2.4moL, 1.1eq) with stirring, and control the reaction temperature to 0°C-40°C; every 30 minutes after 1 hour Take a sample and check the progress of the reaction with gas chromatography until the raw material menthyl lactate cannot be detected. Then add a small amount of hydrazine hydrate with a concentration of 80% to make the reaction solution colorless, continue to stir for 30 minutes and then stand still for layering; separate the separated water phase
[0049] Extract twice with 100 ml of dichloromethane respectively, combine the organic phases, wash twice with 100 ml of water, and then dry the organic phase with magnesium sulfate unt...
Embodiment 2
[0051] Add 300 ml of dichloromethane into a 1000 ml four-necked flask equipped with stirring, thermometer, condenser and constant pressure dropping funnel, and add 600 g of menthyl lactate (2.6moL, 1eq) and 42 g of sodium bromide ( 0.4moL, 0.16eq), after the menthyl lactate is completely dissolved, slowly add 300ml of 27.5% hydrogen peroxide (2.4moL, 0.92eq) with stirring, and control the reaction temperature at 0°C-40°C; every 30 minutes after 1 hour A sample was taken every minute, and the progress of the reaction was checked by gas chromatography until the raw material menthyl lactate could not be detected. Then add a small amount of hydrazine hydrate with a concentration of 80% to make the reaction solution colorless, continue to stir for 30 minutes and then stand still for layering; separate the separated water phase
[0052] Extract twice with 100 ml of dichloromethane respectively, combine the organic phases, wash twice with 100 ml of water, and then dry the organic phase ...
Embodiment 3
[0054] Add 300 ml of dichloromethane into a 1000 ml four-necked flask equipped with stirring, thermometer, condenser and constant pressure dropping funnel, and add 600 g of menthyl lactate (2.6moL, 1eq), 56 g of sodium bromide ( 0.53 mol, 0.2 eq), after the menthyl lactate is completely dissolved, slowly add 300 ml of 27.5% hydrogen peroxide (2.4 mol, 0.92 eq) with stirring, and control the reaction temperature at 0°C-40°C; every 30 minutes after 1 hour A sample was taken every minute, and the progress of the reaction was checked by gas chromatography until the raw material menthyl lactate could not be detected. Then add a small amount of hydrazine hydrate with a concentration of 80% to make the reaction solution colorless, continue to stir for 30 minutes and then stand still for layering; separate the separated water phase
[0055] Extract twice with 100 ml of dichloromethane respectively, combine the organic phases, wash twice with 100 ml of water, and then dry the organic phas...
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