Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Rilpivirine | HCID 6451164 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | Methyl Ethyl Ketone | HCID 6569 | — |
| Product | Rilpivirine hydrochloride | HCID 11711114 | — |
Reaction Steps
Rilpivirine (20 gm; Chromatographic purity: 96.5%) was suspended in a mixture of methanol and methyl ethyl ketone (1:1, 2000 ml) and then heated to reflux for 1 hour to provide a clear solution. The solution was treated with charcoal and filtered through celite bed. The solvent was distilled off under reduced pressure to obtain a residual solid. To the residual solid was added methanol (200 ml) and then heated to 60 to 65° C. To the solution was added a solution of hydrochloric acid in isopropanol (200 ml) at 60 to 65° C. and stirred for 1 hour 30 minutes. The contents were cooled to room temperature and stirred for 30 minutes. The separated solid was filtered and then dried to provide 14 gm of rilpivirine hydrochloride.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09139535B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-83b3be3bfaaa40a09965ecec7c8f2a08 |
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| Source note | uspto-grants-2015_09 |
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