Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Encenicline Hydrochloride | HCID 46208542 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1350343-61-1 | HCID 54597188 | — |
Reaction Steps
The present invention also provides another method for preparing the crystalline Form I, comprising: (a) heating 10-30% by weight of (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride in acetonitrile or an aqueous acetonitrile to between 60° C. and the boiling point of the solution, (b) optionally adding water to the mixture to fully dissolve the (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride; (c) cooling the solution until crystals are just visible; (d) if the water content is greater than 3% volume/volume when crystals are just visible, adding acetonitrile to the mixture so that the water content is less than 3% volume/volume; (e) cooling the resulting mixture to below 15° C.; and (f) isolating crystalline (R)-7-chloro-N-(quinuclidin-3-yl)benzo[b]thiophene-2-carboxamide hydrochloride monohydrate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09273044B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-d1509c5d8c694cf9ad1879b94227988b |
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| Source note | uspto-grants-2016_03 |
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