HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide → N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide | HCID 3009396 | — |
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide hydrochloride | HCID 21995696 | — |
Reaction Steps
In THF (850 ml) was dissolved N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (17.3 g), and to the mixture was added at room temperature 4N hydrochloric acid/ethyl acetate (14 ml). The mixture was stirred for 1 hour. Under reduced pressure, the solvent was evaporated, and the residue was washed with ethyl acetate/acetone and recrystallized from ethanol to give N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide hydrochloride (Compound 112) (11.2 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06235771B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-40d1f96fe6a14c879ed933c474e837e3 |
| Source note | uspto-grants-2001_05 |