Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 9957779 | HCID 9957779 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22727296 | HCID 22727296 | — |
Reaction Steps
A solution of 4-(7-chloro-2H-benzopyran-3-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (95 mg) in acetic anhydride (4 ml) was stirred at 80° C. for 10 hours. The reaction mixture was concentrated and the residue obtained was combined with a 1N aqueous solution of sodium hydroxide and extracted with dichloromethane. The organic phase was washed with aqueous sodium bicarbonate and brine, dried and concentrated to obtain N-[(7-chloro-2H-benzopyran-3-sulfonyl)-2-oxo-1-piperazinyl]-N-[1-(4-pyridyl)-4-piperidinyllacetamide. The resultant free form was dissolved in ethyl acetate, and combined with a solution of hydrochloric acid in ethyl acetate to form a precipitate, which was collected by filtration, washed with ethyl acetate, dried under reduced pressure to obtain the title compound (90 mg) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06723722B1 |
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| Source dataset | uspto-grants-2004_04 |
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| ORD ID | ord-06a4b9edb41247f48c404e051adf4094 |
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| Source note | uspto-grants-2004_04 |
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