Preparation process of thiatro bromoaminium anhydrous compound
A kind of technology of tiotropium bromide and anhydrous, which is applied in the field of preparation of tiotropium bromide anhydrous, and can solve problems such as no tiotropium bromide anhydrous yet.
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[0004] 1. Preparation of Scopolamine (Intermediate 1)
[0005] Take scopolamine hydrobromide, add methanol and potassium carbonate, heat and stir, evaporate to dryness under reduced pressure, add dichloromethane, filter, wash the filter cake three times with dichloromethane, combine the filtrates, dry over anhydrous sodium sulfate, evaporate to dryness under reduced pressure, Obtain scopolamine oil (intermediate one), set aside.
[0006] 2. Preparation of bis(2-thienyl)glycolic acid methyl ester (intermediate 2)
[0007] Take bromothiophene and dissolve it in the ether solution dried by sodium, add dropwise to the ether solution dried by magnesium chips and sodium, after dropping, reflux and cool for later use.
[0008] Take a solution of dimethyl oxalate dissolved in ether, add it dropwise to the above Grignard solution, after dropping, reflux reaction, cool, add dilute sulfuric acid dropwise, separate the ether layer, wash with aqueous sodium carbonate solution, wash with w...
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