HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → Ethyl 3-(2,6-dimethylbenzyloxy)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Ethyl 3-hydroxybenzoate | HCID 24522 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | (2,6-Dimethylphenyl)methanol | HCID 186748 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 3-(2,6-dimethylbenzyloxy)benzoate | HCID 10062422 | — |
Reaction Steps
To a stirred solution of Ethyl 3-hydroxybenzoate (12.21 g, 73.47 mmol) and triphenylphosphine (21.01 g, 80.13 mmol) in dry THF (100 ml) was added dropwise a solution of 2,6-Dimethylbenzyl alcohol (10 g, 73.5 mmol) and diisopropyl azodicarboxylate (16.19 g, 80.13 mmol) in dry THF (35 ml) and dry DMF (15 ml) at ambient temperature. After three hours of stirring at room temperature, the reaction mixture was diluted with diethyl ether and washed twice with water and brine. The combined organic layer was dried over Na2SO4, filtered, concentrated and purified by flash chromatography using ethyl acetate:hexane (1:3) as elutent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932290B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-3e3168dc4c4d441489438cf1ec8d93e9 |
| Source note | uspto-grants-2011_04 |