Preparation method for sodium phenylbutyrate
A technology of sodium phenylbutyrate and phenylbutyric acid, which is applied in the preparation of carboxylate, the preparation of carboxylate, the preparation of organic compounds, etc., can solve problems such as environmental hazards, non-compliance with green environmental protection, and bodily harm to synthetic personnel.
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Embodiment 1
[0052] Embodiment 1, the preparation of methyl 4-phenylbutyrate
[0053] Using industrial grade phenylbutyric acid as raw material, according to figure 1 The scheme shown prepares methyl 4-phenylbutyrate.
[0054] In this example, the raw material industrial grade phenylbutyric acid was purchased from Nanjing Kangmanlin Chemical Industry Co., Ltd., and the purity was 97.5%.
[0055] The consumption of each raw material in this example is shown in Table 1.
[0056] Table 1 methyl phenylbutyrate preparation raw material feed table
[0057]
[0058] like figure 1 As shown, 1000 ml of methanol and 1000 g of technical grade phenylbutyric acid were sequentially put into a 2000 ml four-neck reaction flask, and 50 ml of concentrated sulfuric acid was added after stirring and dissolving. Stir and heat to reflux until the raw material disappears. The reaction was monitored by TLC (developing solvent: ethyl acetate:triethylamine 10:1, raw material Rf=0.2, methyl phenylbutyrate Rf=0...
Embodiment 2
[0062] Embodiment 2, the investigation of methanol consumption in the preparation technology of methyl 4-phenylbutyrate
[0063] The preparation process of methyl 4-phenylbutyrate uses methanol as the reaction solvent, and the present invention investigates the influence of the amount of methanol on the product yield.
[0064] Prepare methyl 4-phenylbutyrate according to the method in Example 1, the reaction conditions are basically the same as in Example 1, the difference is: the consumption of methanol is as shown in Table 3, carried out in parallel six times, under each condition 4- The yield of methyl phenylbutyrate is shown in Table 2.
[0065] As can be seen from the data in Table 3, under the condition that the consumption of phenylbutyric acid and methanol is 1:1 (g / L), 1:1.5 (g / L) and 1:2 (g / L), The yield of methyl 4-phenylbutyrate is basically the same (above 92%), and under the condition of 1:1 (g / L), the yield is basically stable under the condition of enlarging t...
Embodiment 3
[0068] Embodiment 3, the preparation of phenylbutyric acid
[0069] The 4-phenylbutyric acid methyl ester prepared by embodiment 1 is hydrolyzed, acidified to prepare phenylbutyric acid, the flow chart is as follows image 3 shown.
[0070] The consumption of each raw material in this example is shown in Table 4.
[0071] Table 4 phenylbutyric acid preparation raw material feeding table
[0072]
[0073] like image 3 As shown, add 6000 ml of absolute ethanol and 450 g of sodium hydroxide into a 10L four-necked reaction flask in turn, heat to 50-60 °C, stir to dissolve, add 1000 g of methyl 4-phenylbutyrate, and stir to react at 55 °C. The progress of the reaction was monitored by TLC (developing solvent: ethyl acetate:triethylamine 10:1, phenylbutyric acid Rf=0.2, 4-phenylbutyric acid methyl ester Rf=0.75), and the starting material disappeared in 40 minutes.
[0074] Post-treatment: The solvent was distilled off under reduced pressure at 50°C to obtain a white solid. ...
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