Preparation method of levocarnitine intermediate
A technology of intermediate and reaction system, which is applied in the field of preparation of levocarnitine intermediates, can solve the problems of high impurity content, affecting the quality of levocarnitine products, etc., to reduce the impurity content, improve the color of L- nitrile, Improve color effect
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Embodiment 1)
[0018] The preparation method of the levocarnitine intermediate of the present embodiment is as follows:
[0019] ① Add 400g of trimethylamine hydrochloride aqueous solution (2.13mol) with a concentration of 51wt% and 11.8g of trimethylamine aqueous solution (0.05mol) with a concentration of 25wt% into the reaction device, cool down to 5-10°C, and add 130g of S-epichlorohydrin (1.40mol), after dropping, firstly keep the reaction at 5-10°C for 2h, then raise the temperature to 30°C and keep it for 4h.
[0020] After the reaction, 1% phytic acid by weight of the reaction system was added, kept at 30°C for 0.5h, and filtered to obtain a transparent yellow-brown L-quaternary ammonium salt solution.
[0021] ②Heat the L-quaternary ammonium salt solution obtained in step ① to 40-45°C, add 250g of 30wt% sodium cyanide aqueous solution (1.53mol) dropwise, and keep the reaction at 40-45°C for 4h after dropping.
[0022] After the reaction is over, first use hydrochloric acid to adjust...
Embodiment 2~ Embodiment 4)
[0024] The preparation method of each embodiment is basically the same as that of Example 1, the difference lies in the amount of phytic acid added, see Table 1 for details.
[0025] Table 1
[0026]
Embodiment 5~ Embodiment 7)
[0028] The preparation method of each embodiment is basically the same as that of Example 1, the difference lies in the amount of activated carbon added, see Table 2 for details.
[0029] Table 2
[0030]
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