HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 18504646, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | 4-(3,3-Dichloro-2-propenyloxy)-2,6-dichlorophenol | HCID 11346738 | — |
| Reactant | HCID 18504564 | HCID 18504564 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18504646 | HCID 18504646 | 35% |
Reaction Steps
To a mixture of 0.4 g of 2-[2-(4-chlorophenyl)-1,3-dioxolan-4-yl]ethanol, 0.46 g of triphenylphosphine and 6 ml of tetrahydrofuran was added dropwise 0.35 ml of diisopropyl azodicarboxylate, while stirring at room temperature. After further stirring for 15 minutes, a solution of 0.5 g of 4-(3,3-dichloro-2-propenyloxy)-2,6-dichlorophenol in 2 ml of tetrahydrofuran was added. After stirring continued at room temperature for 3 hours, the reaction mixture was concentrated, and the residue was subjected to silica gel chromatography, which afforded 0.3 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-[2-[2-(4-chlorophenyl)-1,3-dioxolan-4-yl]ethoxy]benzene (35% yield), m.p. 84.1° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06268313B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-8e33cad7877d4f5bb434887a2ae859de |
| Source note | uspto-grants-2001_07 |