関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl malonate | HCID 7943 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Bromo-1-fluoro-2-nitrobenzene | HCID 2736328 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 1,3-Dimethyl 2-(4-bromo-2-nitrophenyl)propanedioate | HCID 15740596 | — |
反応手順
To a suspension of NaH (60% in mineral oil, 972 mg, 24.3 mmol) in DMSO (16 mL) is added dimethyl malonate (2.78 mL, 24.3 mmol). The mixture is heated at 60° C. for 10 min and then is cooled to room temperature before 4-bromo-1-fluoro-2-nitro-benzene (1.0 mL, 8.1 mmol) is added. The resulting mixture is heated at 60° C. for 3 hr and then is quenched with saturated aqueous NH4Cl solution. The mixture is extracted with EtOAc, washed with brine, dried over MgSO4, and concentrated. The crude is used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08101608B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-c24f09dbbd18411d807358b383b3f8db |
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| 出典メモ | uspto-grants-2012_01 |
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