참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Nitromethane | HCID 6375 | — |
| 반응물 | Ammonium Acetate | HCID 517165 | — |
| 반응물 | 4-(4-Chloro-3-(trifluoromethyl)phenoxy)benzaldehyde | HCID 86666187 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | (E)-1-Chloro-4-(4-(2-nitrovinyl)phenoxy)-2-(trifluoromethyl)benzene | HCID 67775160 | 99.1% |
반응 단계
To the mixture of 4-(4-chloro-3-(trifluoromethyl)phenoxy)benzaldehyde (600 mg, 1.996 mmol), ammonium acetate (77 mg, 0.998 mmol) in AcOH (5 mL) was added nitromethane (0.323 mL, 5.99 mmol). It was heated at 120° C. for 3 h, then concentrated in vacuo. The residue was dissolved in DCM (30 ml), washed with saturated NaHCO3 aqueous solution (20 ml×2), and brine. The organic phase was collected, dried over Na2SO4, filtered, concentrated to provide the title compound as a brown solid (680 mg, 66.4% yield), which was used without further purification. LCMS: rt=4.17 min, [M+H+]=344.1
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08637536B2 |
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| 출처 데이터셋 | uspto-grants-2014_01 |
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| ORD ID | ord-6fcbf7a1f8794f02bb7ce84bda8dcce2 |
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| 출처 메모 | uspto-grants-2014_01 |
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