Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Piperonylamine | HCID 2723901 | — |
| Reactant | HCID 22611370 | HCID 22611370 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22611528 | HCID 22611528 | 47.2% |
Reaction Steps
To a solution of 5.8 gm (90 mMol) potassium hydroxide in 75 mL methanol were added 9.22 gm (60 mMol) 4-piperidone hydrochloride monohydrate followed by 7.8 gm (30 mMol) 5-(4-fluorobenzoyl)amino-3-(piperidin-4-yl)-1H-indole (Example 182A). This solution was stirred at reflux for 18 hours. The reaction mixture was cooled to ambient and then poured slowly into 150 mL water, maintaining the temperature of the solution at about 20° C. The resulting precipitate was filtered and recrystallized from ethanol to give 4.72 gm (47.2%) of the title compound as tan crystals. 0.725 gm of the material were crystallized again from ethanol to provide 0.241 gm light yellow crystals for analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06380201B1 |
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| Source dataset | uspto-grants-2002_04 |
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| ORD ID | ord-2f39ca2fed154f448169fcbbbcf11281 |
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| Source note | uspto-grants-2002_04 |
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