HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethylphosphine → HCID 57344512, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethylphosphine | HCID 68983 | — |
| Reactant | HCID 86666724 | HCID 86666724 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 57344512 | HCID 57344512 | 45.3% |
Reaction Steps
A round bottomed flask containing crude 4-azido-6-(4-chlorophenyl)-1-methyl-4H-benzo[c]isoxazolo[4,5-e]azepine (1.05 g, 3.0 mmol), was purged with nitrogen and diluted with THF (30 mL) and water (6 mL). Trimethylphosphine (6.03 mL, 6.0 mmol, 1M in toluene) was added dropwise. The solution was stirred at ambient temperature for 2 h. The reaction was poured into half-saturated brine (100 mL), extracted with EtOAc (3×), dried over Na2SO4, filtered, concentrated and purified on a Biotage system (isocratic elution 65% EtOAc: 35% Hexanes) to provide the title compound as an oil (0.44 g). LC/MS m/z 324 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796261B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-faf011a5458a4828a8cc9edaac9ab36f |
| Source note | uspto-grants-2014_08 |