Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 21995795 | HCID 21995795 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21995805 | HCID 21995805 | 51.5% |
Reaction Steps
To a solution of 7-(4-chlorophenyl)-N-[4-[N-(4,4-ethylenedioxycyclohexyl)-N-methylaminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (180 mg) in THF (15 ml) was added at room temperature 3N hydrochloric acid (1 ml), and the mixture was stirred for 7 days. To the mixture was added saturated sodium bicarbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried with magnesium sulfate and concentrated under reduced pressure to give colorless solid, which was recrystallized from ethyl acetate to give colorless crystals of 7-(4-chlorophenyl)-N-[4-[N-methyl-N-(4-oxocyclohexyl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 23) (85.9 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06235771B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-56a3f0f823964112b7e3206bcfe1a3a7 |
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| Source note | uspto-grants-2001_05 |
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