A kind of preparation method of lycopene intermediate
A technology for lycopene and intermediates, which is applied in the field of preparation of lycopene intermediates, can solve the problems of difficult industrialization, a large amount of phosphorus-containing waste water, dangerous DMSO sodium salt, etc., and achieves mild reaction conditions, easy realization, and environmental friendly coefficient. High, simple synthetic route effect
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[0032] A preparation method of a lycopene intermediate, comprising:
[0033] Transesterification reaction step: under alkaline conditions, C5 chloroester and methanol undergo a transesterification reaction to generate C5 chlorohydrin;
[0034] The reaction equation of transesterification reaction step is as reaction formula 3:
[0035]
[0036] Reaction 3
[0037] Phosphine salt reaction step: under the protection of an inert gas, the C5 chlorohydrins obtained in the transesterification step and triphenylphosphine are heated in an alcohol solvent to generate C5 phosphine salt;
[0038] The reaction equation of the phosphonium salt reaction step is as reaction formula 4:
[0039]
[0040] Reaction 4
[0041] Wittig reaction step: under inert gas protection and alkaline conditions, the C5 phosphonium salt obtained in the phosphonium salt reaction step undergoes a Wittig reaction with citral to generate C15 alcohol.
[0042] The reaction equation of the Wittig reaction ...
Embodiment 1
[0055] A preparation method of a lycopene intermediate, comprising:
[0056]Transesterification reaction steps: Add 0.10 mol of sodium hydroxide solid and 1000 ml of methanol into a three-neck flask equipped with a thermometer and magnetic stirring, add 1.0 mol of C5 chloroester after stirring and dissolving, and increase the temperature to 60°C under reduced pressure after the addition, and the system pressure is 600mbar. Methyl acetate and methanol are distilled out quickly, and when the distilled fraction becomes less under the pressure and external temperature, continue to add dropwise 0.02mol sodium hydroxide dissolved in 100ml methanol solution through a 150ml eggplant-shaped dropping funnel, and continue The distillate is distilled under reduced pressure until no distillate is distilled under the pressure and temperature, and the distillation is complete. After cooling down to room temperature, transfer it to a single-necked bottle, concentrate and dry methanol under re...
Embodiment 2
[0060] A preparation method of a lycopene intermediate, comprising:
[0061] Transesterification reaction step: add 0.12mol sodium hydroxide solid and 1200ml methanol into a three-necked flask equipped with a thermometer and magnetic stirring, stir and dissolve, add 1.0mol of C5 chloroester, after the addition, reduce the pressure and heat up to 60°C, the system pressure is 600mbar, methyl acetate and methanol are distilled out quickly, and when the distilled fraction becomes less under the pressure and external temperature, continue to add dropwise 0.01mol sodium hydroxide dissolved in 50ml methanol solution through a 150ml eggplant-shaped dropping funnel, And continue to distill the distillate under reduced pressure until no distillate is distilled under the pressure and external temperature, and the distillation is completed. After cooling down to room temperature, it was transferred to a single-necked bottle, methanol was concentrated and dried under reduced pressure, and ...
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