HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dicyclohexylamine → Dichloro(dicyclohexylamino)phosphine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dicyclohexylamine | HCID 7582 | — |
| Reactant | Phosphorus trichloride | HCID 24387 | — |
| Reactant | Dicyclohexylamine hydrochloride | HCID 2793652 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | Dichloro(dicyclohexylamino)phosphine | HCID 13311825 | 77% |
Reaction Steps
A mixture of 34.4 g (0.25 moles) of PCl3 in 400 mL of hexane was treated with Cy2NH (90.7 g, 0.50 moles) dropwise at ° C. for 30 min. The resulting white slurry was warmed to room temperature and stirred for 1 h, refluxed overnight before removal of Cy2NH—HCl by filtration. The white solids were washed with hexane (2×100 mL). The combined filtrates were concentrated to give the crude Cy2N—PCl2 (54.0 g, 77% yield). 31P NMR (121 MHz, CD2Cl2): δ171.3 (s) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06762330B2 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-6c60c341c08048fa87766dce1af6d968 |
| Source note | uspto-grants-2004_07 |