HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 7-(5-fluoro-2-{[(4-methyl-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-(5-fluoro-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate | HCID 70664967 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 7-(5-fluoro-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 70665371 | — |
Reaction Steps
1,1-dimethylethyl 7-(5-fluoro-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (0.304 g) was dissolved in a minimum amount of dioxane. The solution was cooled in ice and to this was added a solution of HCl in dioxane (2 ml). This was stirred until the reaction had gone to completion by tlc. The reaction mixture was concentrated in vacuo. The product salt was dissolved in water and backwashed with ethyl acetate. The aqueous was neutralised with aqueous sodium hydroxide (1M). This was extracted with ethyl acetate. The organics were dried over sodium sulphate and concentrated to give the title compound, 100 mg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447074B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-c38be5ebcfcc4aeab62dfe3a7066a3cc |
| Source note | uspto-grants-2016_09 |