참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Formamide | HCID 713 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 반응물 | Methanethioamide | HCID 3005587 | — |
| 반응물 | 1-(4-Acetylphenyl)-2-bromo-1-ethanone | HCID 14913299 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | HCID 22316642 | HCID 22316642 | 36% |
반응 단계
To a stirred suspension of phosphorus pentasulfide (24.5 g, 110 mmol) in dioxane (250 ml) was added formamide (28.4 g. 630 mmol), and the mixture was heated at reflux temperature for 2 hours. The reaction mixture was cooled down to room temperature, and the solution was decanted away from solids. To a stirred solution of 1-(4-acetylphenyl)-2-bromo-1-ethanone (2.0 g, 8.3 mmol) in dioxane (80 ml) was added the thioformamide solution, and the mixture was heated at reflux temperature for 13 hours. The reaction mixture was cooled down to room temperature, and made basic by addition of 0.5M NaOH aqueous solution. The whole was extracted with diethylether. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was purified by flash chromatography eluting with ethyl acetate-hexane (1:4) to give the title compound (610 mg, 36% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06949536B2 |
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| 출처 데이터셋 | uspto-grants-2005_09 |
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| ORD ID | ord-460544d78d7c47dd830ec9a862aeb1e4 |
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| 출처 메모 | uspto-grants-2005_09 |
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