関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | 2,2,6,6-Tetramethylpiperidine | HCID 13035 | — |
| 反応物 | 1-Bromo-3,5-bis(trifluoromethyl)benzene | HCID 67602 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Bromo-4,6-bis(trifluoromethyl)benzaldehyde | HCID 86674259 | — |
反応手順
A 2.59 M hexanes solution of n-BuLi (1.13 mL, 2.92 mmol) was added dropwise to a, 0° C., THF solution (4 mL) of 2,2,6,6-tetramethylpiperidine (0.50 mL, 2.92 mmol). After 5 min at 0° C., the solution was cooled to −78° C. and 1-bromo-3,5-bis(trifluoromethyl)benzene was added dropwise over 2 min. The resulting brown amber colored solution was stirred at −78° C. for an additional 20 min. Ethyl formate (0.587 mL, 7.30 mmol) was then added dropwise at −78° C. over 1 min. After 30 min at −78° C., 1 M aqueous HCl was added, the layers were separated and the organic layer was washed with 0.1 M aqueous HCl and 1 M aqueous. The organic layer was dried (Na2SO4), concentrated, and short path vacuum distilled to provide the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08748624B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-9e6e1e238479481e94e033818886ccae |
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| 出典メモ | uspto-grants-2014_06 |
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