Preparation method of ibudilast
A technology of ibudilast and step 2, applied in the preparation field of ibudilast, can solve the problems of difficult operation, low yield, inability to realize large-scale industrial production, etc., and achieves high product purity, high yield, and reduced types and the effect of the quantity used
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specific Embodiment approach 1
[0015] Specific embodiment one: present embodiment is a kind of preparation method of ibudilast, specifically completes according to the following steps:
[0016] 1. First, dissolve hydroxylamine oxysulfonic acid in the solvent, then add 2-picoline dropwise under ice-bath condition, after adding 2-picoline, raise the temperature to 50℃~90℃, and React at ~90°C for 0.5h~1h, then add inorganic base I, and stir at a stirring speed of 100r / min~300r / min until no bubbles are generated, then stir at a speed of 45r / min~90r / min and a temperature of 40 Rotary evaporation method at ℃~60℃ to constant weight, the obtained solid was washed 2 to 3 times with absolute ethanol, the filtrates obtained from the washing were combined, and the inorganic acid was added dropwise at the temperature of -15℃~-10℃ Or carry out acidification treatment with organic acid, the acidification treatment time is 0.5h~1h, and finally filter to obtain 1-amino-2-picoline acid compound;
[0017] 2. First, add 1-ami...
specific Embodiment approach 2
[0023] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the solvent described in step one is selected from deionized water, methylene chloride, benzene, toluene and xylene. Others are the same as in the first embodiment.
specific Embodiment approach 3
[0024] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the inorganic base I described in step one is potassium carbonate, sodium carbonate, sodium hydroxide or potassium hydroxide. Others are the same as in the first or second embodiment.
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