関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Sulfate | HCID 24436 | — |
| 反応物 | 1,2,4-Triacetoxybenzene | HCID 69169 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 1,2,4-Benzenetriol | HCID 10787 | — |
反応手順
Eighty grams of the crude 1,2,4-triacetoxybenzene were dissolved in 200 ml of methanol containing 6 g of concentrated sulfuric acid. The reaction mixture was boiled under reflux for one hour. Then the solution was cooled to room temperature and neutralized with an equivalent amount of fine powdered sodium carbonate. Thereafter 800 ml of ethylether was added whereupon sodium sulfate precipitated out, which was removed by filtration. Reaction by-products and contaminants being responsible for a dark red coloration may be removed employing solid silica gel. After evaporation of the supernatant under reduced pressure, a dark red oil is obtained which crystallized upon standing at 40° C. in the form of a slight reddish solid mass which is pure enough for the next step. This product is 1,2,4-trihydroxybenzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04390559 |
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| 出典データセット | uspto-grants-1983_06 |
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| ORD ID | ord-b3398204d6094d4aac37be2bad88566d |
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| 出典メモ | uspto-grants-1983_06 |
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