Preparation method of calcium alpha-ketoglutarate

Abstract

The invention provides a preparation method of calcium alpha-ketoglutarate, which comprises the following steps: a) adding sodium methoxide into methyl dichloroacetate, and dropwisely adding methyl acrylate to carry out reaction; b) washing the mixed solution in the step a) with water, separating the water phase from the organic phase, and carrying out vacuum distillation on the organic phase to obtain dimethyl 2,2-dichloroglutarate; c) adding NaOH into the dimethyl 2,2-dichloroglutarate, and reacting at 60 DEG C to generate sodium alpha-ketoglutarate; and d) adding calcium chloride into the product in the step c), and stirring to obtain the calcium alpha-ketoglutarate. By changing the addition mode of the catalyst, the catalyst is uniformly distributed in the reaction system; and as the other product is added gradually, the concentration of the catalyst becomes lower, thereby effectively controlling the reaction process between the methyl dichloroacetate and methyl acrylate and enhancing the product yield. The intermediate product can be prepared into the sodium alpha-ketoglutarate by hydrolysis once, thereby shortening the procedure and enhancing the yield.

Description

technical field [0001] The invention belongs to a preparation method of α-ketoglutarate, in particular to a preparation method of calcium α-ketoglutarate. Background technique [0002] Calcium α-ketoglutarate is a white powder, slightly soluble in water, and its chemical formula is C 5 h 4 o 5 Ca, the structural formula is: [0003] [0004] The preparation method of α-ketoglutarate calcium in the prior art is: after mixing methyl dichloroacetate and methyl acrylate, then dropwise adding catalyst sodium methoxide to prepare ketoglutarate dimethyl, the obtained ketoglutarate The acid dimethyl ester is firstly hydrolyzed under acidic conditions, then hydrolyzed under alkaline conditions, and finally reacted with calcium chloride to obtain calcium ketoglutarate. [0005] However, along with the gradual dripping of sodium methylate, the concentration of sodium methylate in the methyl dichloroacetate and methyl acrylate reaction system constantly increases, making the reac...

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Problems solved by technology

[0005] However, along with the gradual dripping of sodium methylate, the concentration of sodium methylate in the methyl dichloroacetate and methyl acrylate reaction system constantly increases, making the reaction between methyl dichloroacetate and methyl acrylate more and more violent, Difficulty controlling the course of the reaction

[0006] Simultaneously, in this reaction, the molar percentage that catalyst occupies relative to reactant is relatively small, in actual reaction process, there may be local sodium methoxide concentration bigger, certainly do not rule out the possibility that local sodium methoxide is smaller, these two Both situations are fatal flaws for this reaction, which will eventually affect the yield and purity of dimethyl ketoglutarate

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