HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 7-[2-({[4-(methyloxy)-2-pyridinyl]methyl}oxy)phenyl]-2,3,4,5-tetrahydro-1H-3-benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,1-dimethylethyl 7-[2-({[4-(methyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70665015 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 7-[2-({[4-(methyloxy)-2-pyridinyl]methyl}oxy)phenyl]-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 70665391 | — |
Reaction Steps
To a stirred solution of 1,1-dimethylethyl 7-[2-({[4-(methyloxy)-2-pyridinyl]methyl}oxy)phenyl]-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.0 g) in dioxane (30 ml) was added hydrogen chloride gas for 2 h at 10-20° C. This was concentrated in vacuo. The residue was dissolved in water, washed with ethyl acetate and basified by adding aqueous sodium bicarbonate. This was extracted with 10% methanol in DCM. The organics were dried over sodium sulphate and concentrated in vacuo to yield the title compound, 2.14 g (91%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447074B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-883733b44cc647f0a4b50898d8eeb5c7 |
| Source note | uspto-grants-2016_09 |