HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylphosphine → HCID 68419400, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylphosphine | HCID 13831 | — |
| Reactant | 1,1'-(Azodicarbonyl)dipiperidine | HCID 73042 | — |
| Reactant | 16-Bromo-1-hexadecanol | HCID 2757013 | — |
| Reactant | 2-(Hexyloxy)phenol | HCID 12413716 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 68419400 | HCID 68419400 | 83.4% |
Reaction Steps
To 350 mL of dehydrated methylene chloride, 12.8 g (66 mmol) of 2-hexyloxyphenol, 23.3 g (73 mmol) of 16-bromohexadecane-1-ol, and 20.0 g (99 mmol) of tri-n-butylphosphine were added. The resulting mixture was cooled with ice under argon. After 25.0 g (99 mmol) of 1,1′-(azodicarbonyl)dipiperidine was added bit by bit while stirring the mixture, 150 mL of methylene chloride was added. Under argon, the mixture was stirred at ambient temperature for 30 minutes and was refluxed for 6 hours. After being cooled, the reaction solution was put into 100 mL of hexane and was filtered. The filtered liquid was purified by silica-gel column chromatography. As a result, 26.5 g of a transparent liquid was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07758932B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-846ddec337684784ae02943f5369d82c |
| Source note | uspto-grants-2010_07 |