Neotame preparation method
A technology of neotame and aspartame, which is applied in the field of preparation of high-intensity sweetener neotame, which can solve the problems of unfavorable industrial production, expensive reducing agent, and high cost, and achieve the effects of quick response, low cost, and convenient operation
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Embodiment 1
[0022] Example 1: Add 300ml of methanol to a 500ml three-necked flask equipped with an electric stirrer and a condensing reflux device placed in a constant temperature water bath, start stirring, add 21.2g of aspartame, stir evenly, add 3,3- Dimethylbutyraldehyde 8.3g, 40°C, reacted for 15min; slowly added 2g of potassium borohydride, kept the temperature at 40°C, reacted for 50min; concentrated under reduced pressure to a thick slurry, added 120ml deionized water, 40°C, hydrolyzed for 1h. Use glacial acetic acid to adjust the pH to 5.5, let it stand to cool to room temperature, put it in the refrigerator (6-8°C) for 12 hours, crystallize, filter with suction, recrystallize the filter cake with methanol aqueous solution with a mass percentage concentration of 20%, and filter with suction , vacuum-dried at 40°C for 12 hours to obtain 19.57g of neotame, with a yield of 71.82%, and a purity of 98.88% by high performance liquid chromatography.
Embodiment 2
[0023] Example 2: The reaction device and operation method were the same as in Example 1, the difference being that the pH of the crystallization was adjusted to 6.5 to obtain 15.30 g of neotame with a yield of 56.15% and a purity of 99.25% by high performance liquid chromatography.
Embodiment 3
[0024] Example 3: The reaction device and operation method are the same as those in Example 1, the difference being that: ① first add 80ml of deionized water to the three-necked flask, preheat to 40°C, start stirring, add 21.2g of aspartame, and stir evenly; ② Add 8.5 g of 3,3-dimethylbutyraldehyde; ③ Add 3 g of potassium borohydride; the result is 20.46 g of neotame, with a yield of 75.08%, and a purity of 99.44% by HPLC.
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