Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86704022 | HCID 86704022 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86704021 | HCID 86704021 | — |
Reaction Steps
To 4-(1-methyl piperidin-4-yloxy)-2-phenyl-9,10-dihydro-4H-3,10a-diaza-benzo[f]azulene-1-carboxylic acid amide (example 254) (250 mg, 0.6 mmole) is added 30% aqueous NaOH solution (2 mL). The reaction mixture is heated to 125° C. overnight. Water (2 mL) is added as well as 1N HCl to pH 6-7. The solvent is removed under reduced pressure. The residue is dissolved in absolute EtOH and filtered to remove inorganic salts. EtOH is removed under reduced pressure. The residue is triturated in Et2O, filtered to afford 4-(1-methylpiperidin-4-yloxy)-2-phenyl-9,10-dihydro-4H-3,10a-diaza-benzo[f]azulene-1-carboxylic acid melting at 185° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09255101B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-ac54f3b2b8394a04bb7c8dcc2a4effa8 |
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| Source note | uspto-grants-2016_02 |
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