関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4,6-Triiodophenol | HCID 11862 | — |
| 反応物 | 1,1'-(3-Bromopropylidene)bisbenzene | HCID 88333 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3,3-Diphenyl-1-(2,4,6-triiodophenoxy)propane | HCID 15343315 | 48.2% |
反応手順
A mixture of 2,4,6-triiodophenol (0.78 g, 1.65 mmol) and potassium carbonate (0.25 g, 1.82 mmol, 1.1 eq) in 5 ml of dimethylformamide was heated at 60° C. for 1 hr, cooled and then 3,3-diphenylpropyl bromide (0.5 g, 1.82 mmol) was added. After stirring for 30 minutes at room temperature the mixture was heated at 60° C. for 24 hrs. The mixture was then cooled, poured into water and the crude product was isolated by ethyl acetate extraction. The product was purified by silica gel chromatography (2.5% ethyl acetate-hexanes) followed by recrystallization from hexanes to give 0.53 g (48%) of a solid. Mp: 120°-121° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05607660 |
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| 出典データセット | uspto-grants-1997_03 |
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| ORD ID | ord-f3bdaa27130a4c3ebdbf3b2397b76b13 |
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| 出典メモ | uspto-grants-1997_03 |
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