HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 54467866, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1,3-Dioxolane | HCID 12586 | — |
| Reactant | (1,3-Dioxolan-2-ylmethyl)triphenylphosphonium bromide | HCID 2724194 | — |
| Reactant | HCID 12987276 | HCID 12987276 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethanamine, 2-(2-methoxyethoxy)-N,N-bis[2-(2-methoxyethoxy)ethyl]- | HCID 112414 | — |
| Product | HCID 54467866 | HCID 54467866 | — |
Reaction Steps
9-Phenyl-9-fluorene carboxaldehyde is dissolved in CH2Cl2 with TDA-1 {tris[2-(2-methoxyethoxy)ethyl]amine} (1 eq). 1,3-dioxolan-2-ylmethyltriphenylphosphonium bromide (1.1 eq) is added followed by a solution of sat. aq K2CO3. The mixture is warmed to reflux and stirred for 15 h. The reaction mixture is diluted with H2O and the resulting mixture is extracted with CH2Cl2. The organic layer is washed consecutively with H2O, 2% aq HCl, and H2O, dried (Na2SO4), and concentrated in vacuo. Purification by liquid chromatography on silica gel affords an E/Z mixture of the dioxolane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06162824 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-4d69f5de95454759b003c903ed0eaab1 |
| Source note | uspto-grants-2000_12 |