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Sodium Hydroxide → 3-(Hexyloxy)-6-hydroxybenzene-1,2-dicarbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,3-Dicyanohydroquinone | HCID 78467 | — |
| 反応物 | Hexyl p-Toluenesulfonate | HCID 220448 | — |
| 生成物 | 3-(Hexyloxy)-6-hydroxybenzene-1,2-dicarbonitrile | HCID 15006689 | 27.5% |
反応手順
11.3 g (44.1 mM) of n-hexyl p-toluenesulfonate was added to the mixture of 5.0 g (31.3 mM) of dicyanohydroquinone and 37.5 ml of 5% NaOH aqueous solution, followed by 7 hours of stirring under refluxing. After the reaction, the reaction mixture was washed with toluene and the aqueous layer was acidified with HCl. The resultant precipitate was recovered through filtration and dried. To the precipitate, 1 liter of toluene was added. After the insoluble substrate was filtered out, the filtrate was subjected to recrystallization in a refrigerator and further subjected to recrystallization from a mixture solvent of water/methanol to obtain 2.1 g of an objective product (yield: 27.5%). m.p.: 150°-153° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05118441 |
| 出典データセット | uspto-grants-1992_06 |
| ORD ID | ord-530bb1a0d7914875b4dc65c98f76c6ee |
| 出典メモ | uspto-grants-1992_06 |