HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → (But-3-yn-2-yloxy) Benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 3-Butyn-2-ol | HCID 16239 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | 1-(3-(1-Hydroxy-1-methylethyl)phenyl)ethanone | HCID 13531419 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (But-3-yn-2-yloxy) Benzene | HCID 12519596 | — |
Reaction Steps
Phenol 27 (422.9 mg, 4.49 mmol), But-3-yn-2-ol (300 mg, 4.28 mmol) were dissolved in anhydrous THF (10 mL) under N2 atmosphere, at 0° C. was added Ph3P (1.12 g, 4.26 mmol) portion wise, stirred it for 10 min, and then DEAD (894.6 mg, 5.14 mmol) added slowly. The resultant solution was heated up to 70° C. stirred for 20 h. To the reaction mixture water added and extracted with DCM and dried organic layer on MgSO4, filtered, concentrated. Purified by flash chromatography using ethylacetate/n-hexane, 5:95) provided compound 28 (450 mg, 69%) as a solid. 1H NMR (CDCl3, 400 MHz) δ 1.67 (d, J=6.8 Hz, 3H), 2.47 (d, J=2 Hz, 1H), 4.88 (q, J=2 Hz, 1H), 6.97-7.03 (m, 3H), 7.28-7.32 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447134B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-c87323b5de76448da663a06fe061e6df |
| Source note | uspto-grants-2016_09 |