참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl triflate | HCID 9526 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Benzonitrile, 4-(trifluoromethyl)- | HCID 67995 | — |
| 반응물 | Propargylamine | HCID 239041 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1,5-Dimethyl-2-(4-trifluoromethylphenyl)imidazole | HCID 19430326 | — |
반응 단계
A mixture of methyl trifluoromethanesulfonate (3.3 ml) and p-trifluoromethylbenzonitrile (5.17 g) was heated at 65° C. for 31/2 hours, then cooled to 5° C. The mixture was then dissolved in 10 ml of acetonitrile, and 2 ml of propargylamine in 10 ml of acetonitrile was added. The mixture was stirred at room temperature for 16 hours, then cooled to 5° C. and 3 ml of concentrated sodium hydroxide added (about 1 equivalent), followed by 40 ml of methylene chloride. The organic layer was separated, the solvent evaporated under reduced pressure, and 50 ml of toluene added. The mixture was refluxed for 3 hours, cooled, the solvent evaporated under reduced pressure, and the residue recrystallized from isopropyl ether, to yield 4.6 g of 1,5-dimethyl-2-(4-trifluoromethylphenyl)imidazole, a compound of Formula (6), m.p. 130° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05428037 |
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| 출처 데이터셋 | uspto-grants-1995_06 |
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| ORD ID | ord-8a361d1bf92d440e8c76e29a51b3f5f0 |
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| 출처 메모 | uspto-grants-1995_06 |
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