HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 18542692, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 2,6-Xylenol, 4-nitro- | HCID 17030 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | Tert-butyl 4-hydroxypiperidine-1-carboxylate | HCID 643502 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18542692 | HCID 18542692 | 71.6% |
Reaction Steps
To a solution of 1-t-butoxycarbonyl-4-hydroxypiperidine (2.40 g), 2,6-dimethyl-4-nitrophenol (1.50 g) and triphenylphosphine (3.06 g) in dichloromethane (60 ml) was added dropwise diethyl azodicarboxylate (1.80 ml) in an ice bath and the mixture was stirred at room temperature for 19 hours. The reaction mixture was concentrated in vacuo. The residue was purified by chromatography on a silica gel column using hexane/ethyl acetate=5/1 as an eluant to give the desired compound (2.25 g, yield 71%) as a colorless solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06555556B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-6aad36520e174e52a1b1d25f2a560e00 |
| Source note | uspto-grants-2003_04 |