関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | (Prop-2-ynyloxy)benzene | HCID 83613 | — |
| 反応物 | Phenyl 5-bromothiophene-3-carboxylate | HCID 58591683 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Phenyl 5-(3-phenoxy-1-propynyl)-3-thiophenecarboxylate | HCID 16220355 | — |
反応手順
A mixture of phenyl 5-bromothiophene-3-carboxylate, Example 113 (100 mg, 0.35 mmol), (prop-2-ynyloxy)benzene (93 mg, 0.71 mmol), triphenylphosphine (19 mg, 0.071 mmol), dichlorobis(triphenylphosphine)palladium(II) (12 mg, 0.018 mmol), copper iodide (1 mg, 0.006 mmol) and triethylamine (0.74 mL, 5.30 mmol) in N,N-dimethylformamide (1 mL) was stirred under nitrogen in a heavy walled process vial in a microwave synthesizer at about 120° C. for about 25 minutes. The reaction mixture was concentrated under vacuum and the residue was purified by flash column chromatography on silica gel using hexane/ethyl acetate (2:1) as the mobile phase to provide the desired product. MS (DCI-NH3): m/z 352 (M+NH4)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07468371B2 |
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| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-8c1c44f128624e6d9e7e013a7fe9f2b8 |
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| 出典メモ | uspto-grants-2008_12 |
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