HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanomethylenetributylphosphorane → HCID 59750743, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| Reactant | HCID 59750809 | HCID 59750809 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 59750743 | HCID 59750743 | 58.1% |
Reaction Steps
In toluene (5 ml) was dissolved 7-[(4-chlorophenyl)sulfonyl]-7-(2,5-difluorophenyl)-1-heptanol (200 mg, 0.496 mmol), followed by the addition of cyanomethylenetri-n-butylphosphorane (400 mg, 1.66 mmol). Under an argon atmosphere, the resulting mixture was heated under reflux for 14 hours. After the reaction mixture was allowed to cool down, the residue obtained by concentrating the reaction mixture under reduced pressure was subjected to flash silica gel chromatography. The fraction obtained from the hexane:ethyl acetate=10:1 eluate was concentrated under reduced pressure to give a white solid. The white solid was washed with hexane, whereby the title compound (111 mg, 0.288 mmol, 58%) was obtained as a white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399775B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-a25ac964db4a46c5b4e7c13d716a9db9 |
| Source note | uspto-grants-2008_07 |