関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1,4-Dibromo-2,5-difluorobenzene | HCID 67596 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 4-Bromo-2,5-difluorobenzaldehyde | HCID 22489081 | 37% |
反応手順
n-Butyl lithium (3.6 ml, 7.7 mmol) was added drop wise to a solution of 1,4-dibromo-2,5-difluoro-benzene (2 g, 7.35 mmol) in dry ether at −78° C. under nitrogen atmosphere and the resulting mixture was stirred at −78° C. for 30 minutes. This was followed by the addition of DMF (0.85 ml, 11.03 mmol) in dry THF. The resultant was stirred at room temperature for 1 hour. The reaction was monitored by TLC (5% ethyl acetate in hexane). The reaction mixture was partitioned between ethyl acetate and saturated ammonium chloride. The organic layer was concentrated and purified by column chromatography on silica gel (2% ethyl acetate in hexane) to afford 600 mg of the product (37% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09029399B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-5f194aae72294b5c9d42b853a801076a |
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| 出典メモ | uspto-grants-2015_05 |
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