Novel method for preparing ademetionine 1,4-butanedisulfonate
A technology of butanedisulfonate and adenosylmethionine, which is applied in the field of preparation of S-adenosylmethionine 1,4-butanedisulfonate, can solve the problem of cumbersome process, poor control of the number and types of impurities, and unfavorable industrial production and other problems, to achieve the effect of high purity, less amount and type of impurities, and fewer synthesis steps
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[0021] Preparation of methylating reagents
[0022] In a 500 mL single-port reaction equipped with magnetic stirring, add dry 180 mL diethylene glycol dimethyl ether and 55 mL dry boron trifluoride ether solution under nitrogen protection, cool to 0°C in an ice bath, and slowly add 41 mL Dry epichlorohydrin, drop over one hour. After the dropwise addition, the temperature was naturally raised to 5-10°C for 5 hours, filtered under nitrogen atmosphere, and the filter cake was washed with anhydrous ether (50 mL×2). After drying with nitrogen, 61 g of methylation reagent was obtained, with a yield of 75%. Store at low temperature (less than -10°C).
[0023] Synthesis of SAMe
[0024] Add 45 ml of trifluoroacetic acid into a 250 mL three-neck flask, cool to -10°C, add 5 g of raw materials under nitrogen protection, add methylation reagent in batches, and complete the addition in one hour, then naturally heat up to 0°C with an ice-salt bath The reaction was monitored by HPLC. A...
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