참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Iodide | HCID 4875 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Picric Acid | HCID 6954 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Bis-(4-chloro-phenyl)-(1H-imidazol-2-yl)-methanol | HCID 12433870 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | HCID 21321305 | HCID 21321305 | — |
반응 단계
To a suspension of 9.6 g (0.030 mol) of α,α-bis(p-chlorophenyl)imidazole-2-methanol (prepared according to Example III) in 100 ml. of acetonitrile, 500 mg of picric acid, 300 mg of potassium iodide and 1.45 g (0.036 mol) of sodium hydroxide were added at 60° C. The reaction mixture was stirred for one hour and then 4.7 g (0.033 mol) of methyl iodide in 25 ml. of acetonitrile were added dropwise at 55° C. The mixture was refluxed for four hours, the solvent was distilled off and the residue was extracted with a mixture of water and diethyl ether. The solid matter was filtered off and the ethereal phase was dried over sodium sulphate and concentrated. Diethyl ether was added to the residue and the solid matter was filtered off. The two portions of solid material were combined and twice crystallised from isopropyl alcohol and twice from toluene and rewashed with petroleum ether (boiling range 60°-80° C.). α,α-Bis(p-chlorophenyl)-1-methylimidazole-2-methanol was obtained. Melting point 190°-191° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04152441 |
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| 출처 데이터셋 | uspto-grants-1979_05 |
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| ORD ID | ord-fa1e8f200d2b431ba484ee83dd61595a |
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| 출처 메모 | uspto-grants-1979_05 |
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