참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrogen Peroxide | HCID 784 | — |
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Trifluoroiodomethane | HCID 16843 | — |
| 반응물 | 6-(Trifluoromethyl)uracil | HCID 233890 | — |
| 촉매 | Bis(eta-cyclopentadienyl) iron | HCID 7611 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 5,6-Bis(trifluoromethyl)uracil | HCID 57693359 | 63% |
반응 단계
0.18 g (1.0 mmol) of 6-trifluoromethyluracil and 0.058 g (0.3 mmol) of ferrocene were weighed and placed in a 50 ml two-neck flask equipped with a magnetic rotor and the atmosphere in the flask was replaced with argon. The following materials were added thereinto: 1.8 ml of dimethyl sulfoxide, 2.0 ml of a 1N dimethyl sulfoxide solution of sulfuric acid, 1.0 ml of a 2.1 mol/l dimethyl sulfoxide solution of trifluoromethyl iodide and 0.2 ml of a 30% hydrogen peroxide aqueous solution. The mixture was stirred at 60 to 70° C. for 20 minutes and then the resulting solution was cooled to room temperature. Formation of 5,6-bis(trifluoromethyl)uracil (19F-NMR yield: 63%) was confirmed by 19F-NMR with 2,2,2-trifluoroethanol as an internal standard. 5,6-Bis(trifluoromethyl)uracil was obtained as a white solid (0.12 g, yield: 48%) by preparative thin-layer chromatography.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07884202B2 |
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| 출처 데이터셋 | uspto-grants-2011_02 |
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| ORD ID | ord-817faa4969df44339474159d858ea492 |
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| 출처 메모 | uspto-grants-2011_02 |
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