참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ethyl formate | HCID 8025 | — |
| 반응물 | 2,2,6,6-Tetramethylpiperidine | HCID 13035 | — |
| 반응물 | 1-Bromo-3,5-bis(trifluoromethyl)benzene | HCID 67602 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Bromo-4,6-bis(trifluoromethyl)benzaldehyde | HCID 86674259 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08748624B2 |
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| 출처 데이터셋 | uspto-grants-2014_06 |
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| ORD ID | ord-9e6e1e238479481e94e033818886ccae |
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| 출처 메모 | uspto-grants-2014_06 |
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