HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxyamine hydrochloride → 7-(1-Hydroxyimino-ethyl)-1,2,4,5-tetrahydro-benzo[d]azepine-3-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | tert-butyl 7-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-3-carboxylate | HCID 18173273 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 7-(1-Hydroxyimino-ethyl)-1,2,4,5-tetrahydro-benzo[d]azepine-3-carboxylic acid tert-butyl ester | HCID 86594168 | 66.5% |
Reaction Steps
7-Acetyl-3-(tert-butyloxycarbonyl)-2,3,4,5-tetrahydro-1H-3-benzazepine (8.9 g, 30.8 mmol) was dissolved in pyridine (30 ml) and hydroxylamine hydrochloride (2.3 g, 33 mmol) was added and the mixture stirred for 2 h at room temperature. The solvent was evaporated and hexane (300 ml) and water (100 ml) were added and the colourless precipitate was filtered and washed with hexane (3×100 ml). The compound was dried in vacuo to give the title compound (6.23 g, 66%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07429579B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-ce4ab795e23b4b43a6a95d6fb5beeca9 |
| Source note | uspto-grants-2008_09 |