Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Duloxetine | HCID 60835 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Duloxetine Hydrochloride | HCID 60834 | — |
Reaction Steps
Duloxetine free base (35 gm) was dissolved in ethyl acetate (500 ml) and the resulting solution was cooled to 5-10° C. To this solution was added to ethyl acetate-HCl solution (about 12%) dropwise in 10-15 minutes. Slowly white solid started to precipitate out. Addition of ethyl acetate-HCl solution was continued till the pH of slurry reached between 2-3. The thick slurry mass was stirred at 15-20° C. for one hour. Solid was filtered, washed with ethyl acetate and dried under reduced pressure at 45-50° C. Yield: 35.3 gm, chemical purity: 99.8% (by HPLC) and chiral purity: 99.95% (by HPLC).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08269023B2 |
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| Source dataset | uspto-grants-2012_09 |
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| ORD ID | ord-0e3df7f2c4ca42b0a1ee23cc5c50b2ef |
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| Source note | uspto-grants-2012_09 |
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