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ChemicalBook CAS DataBase List Tiotropium bromide hydrate
139404-48-1

Tiotropium bromide hydrate synthesis

10synthesis methods
-

Yield:139404-48-1 98%

Reaction Conditions:

in N,N-dimethyl-formamide at 20; for 16 h;Large scale;

Steps:

6 Preparation of tiotropium bromide from N-demethyl-tiotropium

3.6 kg N-demethyl tiotropium was dissolved in 10 L DMF and 2 L methyl bromide was added to the mixture. It was stirred at room temperature for 16 h. The reaction mixture was cooled to 10 °C and diethyl ether was added. Product crystals were filtered and washed with diethyl ether. Wet product was dried under vacuum at 45 °C for 2 h to afford anhydrous tiotropium bromide (4.4 kg of dry product; yield: 98%, HPLC purity: 99.9%)

References:

WO2021/133280,2021,A1 Location in patent:Page/Page column 15

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