참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butyl vinyl ether | HCID 8108 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | N-Methylformanilide | HCID 66737 | — |
| 반응물 | Triphosgene | HCID 94429 | — |
| 용매 | Chlorobenzene | HCID 7964 | — |
| 생성물 | N-Methyl-N-phenylprop-2-enamide | HCID 234887 | — |
반응 단계
To a solution of N-methylformanilide (100 g), butyl vinyl ether (74.12 g) in 85 ml of clorobenzene under stirring at 5° C., a solution of bis-trichloromethylcarbonate (87.84 g) in 170 ml of clorobenzene is added dropwise in 2 hours. The reaction mixture is kept under stirring at room temperature overnight. The mixture is cooled at about 5° C. and the pH is corrected to about 7 by adding sodium hydroxide 15% aqueous solution (348 ml). After separation of the phases, the aqueous layer is extracted with chlorobenzene (90 ml) and the combined organic layers are washed with water (100 ml) and evaporated under reduced pressure. The obtained residue (116.9 g, containing, according to HPLC assay, 104.8 g of pure product, 88% molar yield) is used for the next step of the synthesis without any further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07091382B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-38c716d7c7e943708a6e3647fcb2217f |
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| 출처 메모 | uspto-grants-2006_08 |
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