関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Isobutyraldehyde trimethylsilyl enol ether | HCID 99685 | — |
| 反応物 | Benzyl 4-bromo-3-methoxybenzoate | HCID 58551480 | — |
| 触媒 | Zinc(II) fluoride | HCID 10129912 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzyl 3-methoxy-4-(2-methyl-1-oxopropan-2-yl)benzoate | HCID 86668528 | — |
反応手順
To a flask purged with nitrogen was added Pd(tBu3P)2 (26 mg, 0.050 mmol), ZnF2 (52 mg, 0.50 mmol) and DMF (4 mL). The reaction mixture was allowed to stir for 10 minutes before benzyl 4-bromo-3-methoxy-benzoate (323 mg, 1.01 mmol) was added followed by trimethyl(2-methylprop-1-enoxy)silane (277 μL, 1.51 mmol). The reaction was heated at 80° C. overnight. The crude mixture was quenched with brine and extracted with EtOAc 3 times. The organic layer was dried over sodium sulfate and the solvent was evaporated to give benzyl 3-methoxy-4-(2-methyl-1-oxopropan-2-yl)benzoate. ESI-MS m/z calc. 312.4, found 313.4 (M+1)+; Retention time: 3.27 minutes (4 min run).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08916565B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-a69e54d1aad34fee997f6f535585fb9b |
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| 出典メモ | uspto-grants-2014_12 |
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