- Preparation method of thiobutyrylcholine bromide
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The invention belongs to the field of biochemical detection substrates. The invention relates to a preparation method of thiobutyrylcholine bromide. The method comprises the following steps: (1) dissolving N, N-dimethylaminochloroethane hydrochloride and sodium bicarbonate into 95% ethanol; adding potassium thiobutyrate, reacting at room temperature for 10-12 hours, filtering after the reaction isfinished, concentrating filtrate under reduced pressure to remove ethanol, adding pure water for dispersing, extracting by using ethyl acetate, washing an organic layer by using pure water, drying byusing anhydrous sodium sulfate, concentrating under reduced pressure and distilling, and collecting a fraction at 82-86 DEG C to obtain S-2-(dimethylamino)butyryl mercaptan ethyl ester; and (2) dissolving S-2-(dimethylamino) butyryl mercaptan ethyl ester in ethyl acetate, uniformly stirring, cooling to -5 DEG C, dropwise adding methyl bromide, reacting at -5 DEG C for 4-5 hours, filtering, and drying in a vacuum drying oven for 10-12 hours to obtain white crystal powder. The method has the advantages of low raw material cost, greenness, environmental protection, convenient operation, total yield reaching 75% or above, mild reaction conditions, and suitableness for large-scale production.
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Paragraph 0023-0024; 0026-0027; 0029-0030
(2020/05/08)
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- Synthetic method for s-butyrylthiocholine iodide
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The invention belongs to the technical field of organic synthesis, and provides a synthetic method for s-butyrylthiocholine iodide. The synthetic method comprises the following steps: (1) performing an acylation reaction: performing an esterification reaction on 2-(boc-amino)ethanethiol and butanoyl chloride by using the 2-(boc-amino)ethanethiol as a raw material to obtain s-2-(tert-butoxycarbonylamino)butyryl thiol ethyl ester; (2) performing a deprotection reaction: performing deprotection in the presence of hydrogen chloride by using the s-2-(tert-butoxycarbonylamino)butyryl thiol ethyl ester as a raw material to obtain s-2-aminobutyryl thiol ethyl ester hydrochloride; (3) performing a methylation reaction: performing a reductive amination reaction on the s-2-aminobutyryl thiol ethyl ester hydrochloride and formaldehyde by using the s-2-aminobutyryl thiol ethyl ester hydrochloride as a raw material to obtain s-2-(dimethylamino) butyryl thiol ethyl ester; and 4) performing a quaternization reaction: performing a reaction on the s-2-(dimethylamino) butyryl thiol ethyl ester and iodomethane by using the s-2-(dimethylamino) butyryl thiol ethyl ester as a raw material to obtain the s-butyrylthiocholine iodide. The synthetic method provided by the invention has simple operation, a higher yield and lower costs, and is green, environmentally friendly and suitable for mass preparation.
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Paragraph 0035; 0036; 0037
(2018/10/11)
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