517-23-7Relevant articles and documents
Application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and synthesis method of alpha-acetyl-gamma-butyrolactone
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Paragraph 0085-0106, (2021/05/08)
The invention provides application of liquid sodium methoxide in synthesis of alpha-acetyl-gamma-butyrolactone and a synthesis method of the alpha-acetyl-gamma-butyrolactone, and relates to the technical field of organic synthesis. The synthesis method of the alpha-acetyl-gamma-butyrolactone comprises the following steps: (a) performing pre-acylation reaction on an acetate compound and gamma-butyrolactone; (b) adding liquid sodium methoxide into the reaction liquid in the step (a) to carry out mixed reaction; (c) after the reaction in the step (b) is finished, concentrating and collecting methanol, and transferring the concentrated reaction liquid into an acylation kettle; (d) supplementing the acetate compound into the acylation kettle for acylation reaction; (e) performing neutralizing, filtering and concentrating to obtain an alpha-acetyl-gamma-butyrolactone crude product. According to the method, liquid sodium methoxide is used for replacing solid sodium methoxide for acylation synthesis, so that liquification and sealing of feeding are realized, the on-site feeding risk is reduced, and the synthesis yield is increased to 96% or above.
Process for dissociating acetamidine hydrochloride with alpha-acetyl-gamma-butyrolactone sodium salt
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Paragraph 0064-0120, (2019/03/25)
The invention relates to the technical field of vitamin B synthesis intermediates, in particular to a process for dissociating acetamidine hydrochloride with alpha-acetyl-gamma-butyrolactone sodium salt. The process comprises the following steps: making alpha-acetyl-gamma-butyrolactone sodium salt react with the acetamidine hydrochloride and separating products to obtain acetamidine and alpha-acetyl-gamma-butyrolactone. According to the process, the intermediate product alpha-acetyl-gamma-butyrolactone sodium salt in the synthesis step of the alpha-acetyl-gamma-butyrolactone reacts with the acetamidine hydrochloride, the alpha-acetyl-gamma-butyrolactone sodium salt utilize hydrochloric acid coordinated in the acetamidine hydrochloride to achieve the effect that the alpha-acetyl-gamma-butyrolactone sodium salt produces the alpha-acetyl-gamma-butyrolactone, and the hydrochloric acid in the acetamidine hydrochloride is removed to form acetamidine. Synchronous production of two target products is achieved, the steps are saved, and the process is environmentally friendly and increases the revenue.
Synthesis method for alpha-acetyl gamma-butyrolactone
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Paragraph 0022-0047, (2018/04/21)
The invention relates to the field of synthesis of organic intermediates of prothioconazole, in particular to a synthesis method for alpha-acetyl gamma-butyrolactone. The synthesis method includes thefollowing steps of (1) slowly heating a reactor to 75 DEG C, and adding gamma-butyrolactone, ethyl acetate and sodium ethoxide for reflux reaction for 10 hours to obtain a sodium salt of alpha-acetylgamma-butyrolactone and a by-product ethanol; (2) distilling the product obtained in the step (1) to remove the ethanol and excess ethyl acetate, adjusting the pH of the residue to 3-4 with dilute sulfuric acid, standing for liquid separation, removing aqueous phase, and performing vacuum distillation in an organic phase at a pressure of 0.1 MPa and a temperature of 65-70 DEG C to obtain alpha-acetyl gamma-butyrolactone. The synthesis method uses a reaction base material ethyl acetate as a base solvent and uses sodium ethoxide as a condensing agent, has mild reaction conditions and improved safety, avoids pollution caused by adopting additional solvents such as benzene solvent and the like, and has good safety, simple post-treatment method, high yield of alpha-acetyl gamma-butyrolactone above 90%, and high purity of alpha-acetyl gamma-butyrolactone above 98%.