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 | 3-Iodophenol | HCID 12272 | — |
| 反応物 | 6-(2,4,6-Triiodophenoxy)-1-chlorohexane | HCID 15224801 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(3-Iodophenoxy)-6-(2,4,6-triiodophenoxy)-hexane | HCID 15224802 | 54% |
反応手順
A mixture of potassium carbonate (3.0 g, 21.9 mmol, 1.1 eq), 3-iodophenol (4.4 g, 19.9 mmol) and 6-(2,4,6-triiodophenoxy)-1-chlorohexane (11.75 g, 19.9 mmol) in 50 ml of DMF was heated to 110° C. for 1.5 hours and then cooled. The mixture was poured into water and extracted with ethyl acetate. The organic layer was dried (magnesium sulfate) and evaporated to give a solid which was filtered through basic alumina (hexanes-ethyl acetate). The filtrate was concentrated under vacuum leaving the crude product as a solid. Recrystallization from cyclohexane afforded 8.29 g (54%) of the desired product after drying at room temperature under high vacuum, mp 65-66° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05348727 |
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| 出典データセット | uspto-grants-1994_09 |
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| ORD ID | ord-a886e235efb94f53a82a08847f56a7a8 |
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| 出典メモ | uspto-grants-1994_09 |
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