참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Potassium perfluorobutanesulfonate | HCID 23675274 | — |
| 반응물 | (4-Methylphenyl)(4'-isobutylphenyl)iodonium hydrogensulfate | HCID 86591397 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 18362461 | HCID 18362461 | 34.6% |
반응 단계
4.5 g of potassium nonaflate is suspended in 15 ml of water. To the solution is added 4.93 g of the crude (4-methylphenyl)(4′-isobutylphenyl)iodonium hydrogensulfate dissolved in 10 ml of methanol. The mixture is stirred for 1 hour at room temperature. 15 ml of methylene chloride is added to the solution and stirred overnight at room temperature. The product is extracted with methylene chloride and the organic layer is washed with water, dried over MgSO4, and concentrated. The residue is purified by flash chromatography on silica gel with methylene chloride and ethanol (95:5) as eluent, yielding 2.46 g (3.8 mmol; 34%) of (4-methylphenyl)(4′-isobutylphenyl)iodonium nonaflate as a brown resin. The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ [ppm]: 0.88 (d, 6H), 1.84 (m,1H), 2.41 (s, 3H), 2.50 (d, 2H), 7.21-7.26 (m, 4H), 7.84 (d, 4H). Elemental analysis: calculation for C21H20O3F9SI
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06306555B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_10 |
|---|
| ORD ID | ord-b1f4c4838e314a28833b44c048f8935a |
|---|
| 출처 메모 | uspto-grants-2001_10 |
|---|