94088-03-6Relevant articles and documents
Preparation method of thiobutyrylcholine bromide
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Paragraph 0023; 0025; 0026; 0028; 0029; 0031, (2020/05/08)
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.
