Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 3-Butyn-1-OL | HCID 13566 | — |
| Reactant | HCID 17755957 | HCID 17755957 | — |
| Catalyst | Triphenylphosphine | HCID 11776 | — |
| Catalyst | Palladium Chloride | HCID 24290 | — |
| Catalyst | Copper iodide | HCID 83717 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 17756178 | HCID 17756178 | 45.2% |
Reaction Steps
To a slurry of 2-(4 iodo-benzyl)-isoindole-1,3-dione (2.0 g, 5.51 mmol), triphenylphosphine (14.4 mg, 0.055 mmol), and palladium chloride (5 mg, 0.028 mmol) in DEA (20 mL) was added DMF (4 mL) and copper iodide (11 mg, 0.055 mmol) followed by 3-butyn-1-ol (417 μL, 5.51 mmol). The reaction stirred at room temperature overnight under nitrogen atmosphere. The next day, the reaction mixture was concentrated and purified by flash column chromatography (2:1 Hexane:ethyl acetate) to yield the product as a yellow solid (0.76 g, 45% yield). 1H NMR (600 MHz, CDCl3): δ 7.86 (m, 2H), 7.76 (m, 2H), 7.36 (s, 4H), 4.83 (s, 2H), 3.80 (q, 2H, J=6.3 Hz), 2.68 (t, 2H, J=6.2 Hz), 1.80 (t, 1H, J=6.4 Hz); 13C NMR (150 MHz, CDCl3): δ 167.5, 135.5, 133.6, 131.5, 131.4, 128.0, 122.9, 122.5, 86.3, 81.5, 60.6, 40.8, 23.3.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07485283B2 |
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| Source dataset | uspto-grants-2009_02 |
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| ORD ID | ord-ffb43fcb097849a087377209c84298d7 |
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| Source note | uspto-grants-2009_02 |
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