関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Vanillin | HCID 1183 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,10-Dibromodecane | HCID 221483 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,10-Di(2-methoxy-4-formylphenoxy)decane | HCID 19795109 | — |
反応手順
A slurry of 13.42 g of vanillin, 11.99 g of 1,10-dibromodecane, 6.16 g of anhydrous potassium carbonate and 300 ml of acetone was refluxed with stirring for 48 h, cooled and diluted with 400 ml of water. After the salts had dissolved, the mixture was chilled overnight at 5° C. The solid product was filtered, washed twice with water and recrystallized (still wet) from 250 ml of ethanol. Cooling to 25° C. gave 4.75 g of compound mp 93°-102° C., wetting at 65° C. (Further cooling of the mother liquors to 5° C. furnished 3.5 g of very impure materials, mp 55°-65° C.). Another recrystallization from 130 ml of ethanol raised the mp to 103°-105° C., slight wetting at 99° C.; 3.16 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05247055 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-71e3ae6057b24905aebe514e2d6cc7ed |
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| 出典メモ | uspto-grants-1993_09 |
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