関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Succinic anhydride | HCID 7922 | — |
| 反応物 | 1,3-Benzenediol, 4-methyl- | HCID 10333 | — |
| 生成物 | 9-Carboxyethylidene-3,6-dihydroxy-2,7-dimethyl-9H-xanthene | HCID 19958020 | 74.2% |
反応手順
4-Methylresorcinol (25.8 g, 0.208 mol) and succinic anhydride (20.8 g, 0.208 g) were placed in a round bottom flask and the flask was purged with nitrogen. Methanesulfonic acid (150 mL) was added and the solution heated under nitrogen to 65° C. for 2 hours. The solution was added dropwise to 1 L of rapidly stirred, ice-cooled water with the simultaneous addition of 50% aq sodium hydroxide to maintain the pH at 2.25 +/-0.25. The product was collected by centrifugation and washed with water (3×) and acetone (2×). The solid was air-dried, then vacuum-dried at 110° C. to afford a brick-red powder (24.1 g, 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05242796 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-97f438e7ffbd4764b1ee7bf05860487d |
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| 出典メモ | uspto-grants-1993_09 |
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