関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | 2-Bromo-N-methoxy-N,5-dimethylbenzamide | HCID 53416697 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-5-methylbenzaldehyde | HCID 11845896 | 99% |
反応手順
Step AI (2): 2-Bromo-N-methoxy-N,5-dimethylbenzamide (656 mg, 2.54 mmol) was dissolved in THF (20 mL). The reaction mixture was cooled down to −78° C. and a 1.0M solution of DIBAL-H (7.62 mL, 7.62 mmol) was added. The reaction mixture was stirred at −78° C. for 1 h. The reaction was quenched with acetone and stirred at rt with Rochelle's salt. The mixture was extracted with DCM. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuum to yield 2-bromo-5-methylbenzaldehyde (500 mg, 99%) as a colorless oil. LC-MS (M+H)+=199.21.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772221B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-6006656d4a0b46e5a31a75ba3e62c9e5 |
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| 出典メモ | uspto-grants-2010_08 |
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