HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → 2-[2-[(2-Nitrophenyl)methyl]3-thienyl]-1,3-dioxolane
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | alpha-Bromo-2-nitrotoluene | HCID 77569 | — |
| Reactant | 2-(Tributylstannyl)-3-thienyl-1,3-dioxolane | HCID 11134058 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2-[2-[(2-Nitrophenyl)methyl]3-thienyl]-1,3-dioxolane | HCID 11130065 | — |
Reaction Steps
A mixture of 2-[2-(tributylstannyl)-3-thienyl]-1,3-dioxolane (8.8 gms, 20 mmols), 2-nitrobenzyl bromide (4.5 gms, 22 mmol) and tetrakis (triphenylphosphine)-palladium (0) (200 mg) is refluxed in degassed toluene for 16 hours under nitrogen atmosphere. At the end, the reaction mixture is cooled to room temperature and filtered through diatomaceous earth. The toluene is removed by concentrating at reduced pressure and the product isolated by silica gel column chromatography by elution with 30% ethyl acetate:hexane to give 4.5 gms. of the desired product as a viscous liquid. Mass Spectrum; M+ 292.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05869483 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-10821f3fd9a049049905da95dec329a0 |
| Source note | uspto-grants-1999_02 |