HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 8-Bromo-octanoic acid benzyloxyamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyloxyamine hydrochloride | HCID 102312 | — |
| Reactant | Bis(2-oxo-3-oxazolidinyl)phosphinic chloride | HCID 152842 | — |
| Reactant | 8-Bromooctanoic acid | HCID 548275 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 8-Bromo-octanoic acid benzyloxyamide | HCID 11336403 | 78% |
Reaction Steps
In an ice bath, 14 ml triethylamine was added to a suspension of 3.2 g (20 mmol) O-benzylhydroxylamine hydrochloride in 150 ml dichloromethane. Stirring was continued until the solution became clear. Then, 4.5 g (20 mmol) 8-bromo octanoic acid was added, followed by 5.6 g (22 mmol) bis-(2-oxo-3-oxazolidinyl)-phosphorylchloride. Stirring was continued at ambient temperature for 18 h. The solution was extracted twice with 150 ml each of 1M aqueous hydrochloric acid and twice with 150 ml each of 1M aqueous sodium bicarbonate. The organic solvent was removed i. vac. to give 5.1 g (78%) of 8-bromo-octanoic acid benzyloxyamide as a colorless oil. MS: 330 (M+H+)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07091229B2 |
| Source dataset | uspto-grants-2006_08 |
| ORD ID | ord-1345b2679a1f4255af5f660665af3050 |
| Source note | uspto-grants-2006_08 |