関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Picric Acid | HCID 6954 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bis-(4-chloro-phenyl)-(1H-imidazol-2-yl)-methanol | HCID 12433870 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 21321305 | HCID 21321305 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04152441 |
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| 出典データセット | uspto-grants-1979_05 |
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| ORD ID | ord-fa1e8f200d2b431ba484ee83dd61595a |
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| 出典メモ | uspto-grants-1979_05 |
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