참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Ethyl trifluoroacetate | HCID 9794 | — |
| 반응물 | 2,4-Difluoroacetophenone | HCID 67770 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 4-(2,4-Difluorophenyl)-1,1,1-trifluoro-4-hydroxy-3-buten-2-one | HCID 69934778 | 97.4% |
반응 단계
To a solution of 40.0 g (0.256 moles) 2',4'-difluoroacetophenone (commercially available) in 400 mL diethyl ether at 0° C. was added 40 mL (0.405 moles) ethyl trifluoroacetate. At 5° C., 80 mL of a 25% wt. sodium methoxide in methanol (0.37 moles) were added over 15 minutes. The reaction mixture was stirred overnight at 25° C. The mixture was poured over 300 mL ice water and 21.3 mL (0.37 moles) acetic acid were added. The organic layer was washed two times with water, dried over anhydrous MgSO4, and concentrated in vacuo to give 62.85 g (97%) 4-(2,4-difluorophenyl)-1,1,1-trifluoro-4-hydroxy-3-buten-2-one as a yellow oil; 1HNMR (CDCl3) ppm: 6.61 (s,1H), 6.87 (m,1H), 6.97 (m,1H), 7.97 (m,1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05281571 |
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| 출처 데이터셋 | uspto-grants-1994_01 |
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| ORD ID | ord-ba3f26706658454daba0b17a8d1801b1 |
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| 출처 메모 | uspto-grants-1994_01 |
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