HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanomethylenetributylphosphorane → HCID 59750738, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| Reactant | HCID 59750752 | HCID 59750752 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 59750738 | HCID 59750738 | 64% |
Reaction Steps
In toluene (50 ml) was dissolved 2-[3-[(4-chlorophenyl)sulfonyl]-3-(2,5-difluorophenyl)propylthio]ethanol (800 mg, 2.00 mmol), followed by the addition of cyanomethylenetri-n-butylphosphorane (1.50 g, 6.22 mmol). Under an argon atmosphere, the resulting mixture was heated under reflux for 14 hours. After the reaction mixture was allowed to cool down, it was concentrated under reduced pressure. The residue was subjected to flash silica gel chromatography, and the fraction obtained from the hexane:ethyl acetate=15:1 eluate was concentrated under reduced pressure to give a white solid. The white solid was washed with hexane, whereby the title compound (504 mg, 1.28 mmol, 64%) 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-87619fec0ec3486eaab777853e9737a4 |
| Source note | uspto-grants-2008_07 |