HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 12401049, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 18519030 | HCID 18519030 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 12401049 | HCID 12401049 | — |
Reaction Conditions
| Temperature | -40 °C |
|---|
Reaction Steps
To 2-(3-hydroxy-propylsulfanyl)-phenol (29.2 g, 158.5 mmol) in THF (450 mL) was added triphenylphosphine (52.0 g, 200.0 mmol). The solution was cooled to −40° C. and diethyl azodicarboxylate (31.5 mL, 164.0 mmol) was added slowly. The solution was warmed to rt and stirred for 2.5 h. The THF was removed by evaporation and the residue was treated with 1 L of Et2O. The formed solids were filtered off, and the filtrate concentrated to an oil which was purified over silica gel (10% Et2O/hexane) to a pink oil (16.2 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06576766B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-dd264cd17c424f878120310db6af2635 |
| Source note | uspto-grants-2003_06 |