Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 21995793 | HCID 21995793 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21995796 | HCID 21995796 | 61.2% |
Reaction Steps
To a solution of N-[4-[N-(4,4-ethylenedioxycyclohexyl)-N-methylaminomethyl]phenyl]-7-(3,4-methylenedioxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (100 mg) in THF (10 ml) was added at room temperature 3N hydrochloric acid (1 ml), and the mixture was stirred for 39 hours. 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 were recrystallized from ethyl acetate to give colorless crystals of 7-(3,4-methylenedioxyphenyl)-N-[4-[N-methyl-N-(4-oxocyclohexyl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 21) (56.8 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06235771B1 |
|---|
| Source dataset | uspto-grants-2001_05 |
|---|
| ORD ID | ord-89f508d6e11a4c24b2bf0795d8f247ac |
|---|
| Source note | uspto-grants-2001_05 |
|---|