Tiotropium bromide hydrate synthesis
- Product Name:Tiotropium bromide hydrate
- CAS Number:139404-48-1
- Molecular formula:C19H22BrNO4S2.H2O
- Molecular Weight:490.43
136310-64-0
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139404-48-1
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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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1336913-22-4
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139404-48-1
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1374772-94-7
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1508-46-9
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139404-48-1
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26447-85-8
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155-41-9
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139404-48-1
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411207-31-3
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139404-48-1
284 suppliers
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