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
12.8 g (66 mmol) of 2-hexyloxyphenol, 23.3 g (73 mmol) of 16-bromohexadecan-1-ol and 20.0 g (99 mmol) of tri-n-butylphosphine were added to 350 mL of dehydrated methylene chloride followed by cooling with ice in the presence of argon. After adding 25.0 g (99 mmol) of 1,1′-(azodicarbonyl) dipiperidine a little at a time while stirring, 150 mL of methylene chloride were added. After stirring for 30 minutes at room temperature in the presence of argon, the reaction solution was refluxed for 6 hours. After cooling, the reaction solution was dropped into 100 mL of hexane and filtered. The filtrate was concentrated and purified by silica gel column chromatography to obtain 26.5 g of a clear liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07658979B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-a9a844d735ff48ecbe1a10a69da6dc70 |
| Source note | uspto-grants-2010_02 |