関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclobutanone | HCID 14496 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | 1-Bromo-2-fluoro-4-iodobenzene | HCID 2725006 | — |
| 反応物 | HCID 178418918 | HCID 178418918 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 86698600 | HCID 86698600 | 91% |
反応手順
To 1-bromo-2-fluoro-4-iodobenzene (2390 mg, 7.90 mmol) in tetrahydrofuran (20 mL) at −40° C. was added isopropyl magnesium chloride.lithium chloride (1.3M in THF, 6.4 mL, 5.1 mmol) dropwise. The reaction mixture was stirred at −40° C. for 10 minutes, and treated with additional isopropyl magnesium chloride.lithium chloride (1.3M in THF, 1 mL, 1.3 mmol). The reaction mixture was stirred at −40° C. for an additional 20 minutes and then treated with cyclobutanone (624 mg, 8.72 mmol) dropwise at −40° C. The reaction mixture was warmed to room temperature, and stirred at room temperature for 16 hours. The reaction mixture was quenched with water and extracted with ethyl acetate (3×240 mL). The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo to afford the title compound (1.7 g, 91%) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08889730B2 |
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| 出典データセット | uspto-grants-2014_11 |
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| ORD ID | ord-1c1a93f7db1241e9a7e46fefedb231b0 |
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| 出典メモ | uspto-grants-2014_11 |
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