Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Reactant | HCID 21108270 | HCID 21108270 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 21108374 | HCID 21108374 | 54.7% |
Reaction Steps
A solution of 4-[4-(4-chlorophenyl)-1-piperidinyl]-1-(3-isopropyl-2,3,4,5-tetrahydro-1H-3-benzazepin-7-yl)-4-oxo-1-butanol (0.14 g, 0.30 mmol) obtained in Example 212 and p-toluenesulfonic acid monohydrate (0.03 g, 0.16 mmol) in toluene (10 mL) was refluxed for 24 hours under heating. The reaction solution was concentrated under reduced pressure, and the resultant residues were purified by alumina column chromatography (developing solvent; hexane:ethyl acetate=1:1), whereby 0.09 g free base of the title compound was obtained as colorless amorphous powder. The resultant powder was dissolved in ethyl acetate and treated with 4 N hydrochloric acid in ethyl acetate under cooling with ice-bath, whereby 0.04 g of the title compound was obtained as colorless amorphous powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07229986B2 |
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| Source dataset | uspto-grants-2007_06 |
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| ORD ID | ord-cb682bf7276f42a4a1f4a7a656ce3bcd |
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| Source note | uspto-grants-2007_06 |
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