HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 7-(3-{[(4-ethyl-2-pyridinyl)methyl]oxy}-6-methyl-2-pyridinyl)-2,3,4,5-tetrahydro-1H-3-benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,1-dimethylethyl 7-(3-{[(4-ethyl-2-pyridinyl)methyl]oxy}-6-methyl-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70665117 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 7-(3-{[(4-ethyl-2-pyridinyl)methyl]oxy}-6-methyl-2-pyridinyl)-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 70665374 | — |
Reaction Steps
To a stirred solution of 1,1-dimethylethyl 7-(3-{[(4-ethyl-2-pyridinyl)methyl]oxy}-6-methyl-2-pyridinyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (4.3 g) in dioxane (30 ml) was passed through HCl (gas) for 30 min at 20° C. After completion of reaction by TLC, the solvent was removed in vacuo. The solid obtained was washed with acetone and dissolved in water. This was neutralised with sodium bicarbonate, extracted with DCM and concentrated in vacuo to give a crude product. This was purified through silica using 6% methanol in DCM. Appropriate fractions were combined and concentrated in vacuo to give a product. This was triturated in diethyl ether to yield the title compound, 1.5 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447074B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-b7cbf5c1cbee408a8ca149e0facfde6b |
| Source note | uspto-grants-2016_09 |