Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl trifluoroacetate → 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl trifluoroacetate | HCID 9794 | — |
| 반응물 | 2-Acetylpyridine | HCID 14286 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 4,4,4-Trifluoro-1-(pyridin-2-yl)butane-1,3-dione | HCID 2771478 | 81.2% |
반응 단계
Trifluoro-acetic acid ethyl ester (9.82 mL, 82.5 mmol) was added to a solution of 1-pyridin-2-yl-ethanone (5.00 g, 41.2 mmol) in methanol (40 mL) containing sodium methoxide (61.8 mmol). The reaction mixture was heated at reflux overnight, concentrated under reduced pressure and acidified with aqueous hydrochloric acid (10%). The aqueous solution was extracted with ethyl acetate (10×50 mL). The organic layers were collected, dried over sodium sulfate, filtered, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel to give 4,4,4-trifluoro-1-pyridin-2-yl-butane-1,3-dione (7.26 g, 81%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07098335B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-041f2cc851b84257b82bcd81cc91efb6 |
| 출처 메모 | uspto-grants-2006_08 |