참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Ethyl (dimethoxyphosphinoyl)acetate | HCID 67555 | — |
| 반응물 | 2,4,6-Trifluorobenzaldehyde | HCID 521845 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | tetrahydrofuran N,N-dimethylformamide | HCID 21974620 | — |
| 생성물 | 3-(2,4,6-Trifluoro-phenyl)-acrylic acid ethyl ester | HCID 57412779 | 87% |
반응 단계
To the solution of ethyl[bis(methyloxy)phosphoryl]acetate (1.980 mL, 11.99 mmol) in THF-DMF (60 mL, v/v=5:1) at 0° C. was added t-BuOK (1.458 g, 12.99 mmol) portion wise. The resultant mixture was stirred at room temperature for 30 minutes, then mixed with a solution of 2,4,6-trifluorobenzaldehyde (1.6 g, 9.99 mmol) in THF (10 mL) at 0° C. It was allowed to warm to room temperature and the mixture was stirred for 45 min. It was mixed with aqueous ammonium chloride and then extracted with ethyl acetate. The organic layer was washed with brine, dried over Na2SO4, filtered, and concentrated. The residue was purified by a flash column chromatography to give the title compound as a pale yellow oil (2.0 g, 87% yield). LCMS: rt=3.52 min, [M+H+]=231.1
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-e0957e9540054c5f81479c9091b0c6c2 |
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| 출처 메모 | uspto-grants-2014_01 |
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