関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 4-Fluoro-2-hydroxybenzaldehyde | HCID 2779268 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Bromo-4-fluoro-2-hydroxybenzaldehyde | HCID 7172128 | 17% |
反応手順
Into a 20-L 4-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen was placed a solution of 4-fluoro-2-hydroxybenzaldehyde (545 g, 3.89 mol, 1.00 equiv) in AcOH (5 L), followed by the addition of Br2 (623 g, 3.90 mol, 1.00 equiv) dropwise with stirring at 0-5° C. The resulting solution was stirred overnight at room temperature, quenched by the addition of 3 L of saturated aqueous Na2SO3 and diluted with 6 L of ice/water. The solids were collected by filtration, washed with 2×1.5 L of water and dried to afford 145 g (crude) of 5-bromo-4-fluoro-2-hydroxybenzaldehyde as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09034866B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-01a57c2642fb4febb7760ff1e208e1a8 |
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| 出典メモ | uspto-grants-2015_05 |
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