関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Methylbut-1-yne | HCID 69019 | — |
| 反応物 | Ethyl 3-amino-4-iodobenzoate | HCID 59762281 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 触媒 | HCID 178418476 | HCID 178418476 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Ethyl3-Amino-4-(3-methylbut-1-ynyl)benzoate | HCID 59762350 | — |
反応手順
To a solution of ethyl3-amino-4-iodobenzoate (Compound 31, 6.87 g, 23.1 mmol) in triethylamine (50 ml) at 25° C. under argon then added CuI (22 mg, 1.16 mmol), Pd(PPh3)2Cl2 (82 mg, 1.16 mmol), and 3-methyl-1-butyne ( 3.18 g, 46.2 mmol). The reaction was stirred for 20 h at 25° C., filtered off brown solid, and then rinsed solid with EtOAc, organic layer was concentrated in vacuo. The residue was purified by chromatography on silica gel (0→25% EtOAc-hexanes) to yield the title compound as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524917B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-8cfdaf0063bc4f8ba461f5f905e1d324 |
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| 出典メモ | uspto-grants-2013_09 |
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