関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Resorcinol | HCID 5054 | — |
| 反応物 | Succinic anhydride | HCID 7922 | — |
| 生成物 | 9-(Carboxyethylidene)-3,6-dihydroxy-9H-xanthene | HCID 19958004 | 88.4% |
反応手順
Resorcinol (33.0 g, 0.300 mol) and succinic anhydride (30.0 g, 0.300 mol) were placed in a round bottomed flask and purged with nitrogen. Methanesulfonic acid (150 mL) was added and the solution was stirred at 65° C. for 2 hours under an atmosphere of nitrogen. The reaction mixture was added dropwise to rapidly stirred, ice-cooled water (1 L) with simultaneous addition of 50% aqueous sodium hydroxide to maintain pH 2.5 +/0.5. The product which appeared as a granular precipitate was collected by filtration and rinsed with water (3×100 mL) then acetone (3×100 mL). The product was air-dried then vacuum-dried (vacuum oven) at 110° C. for 18 hours to afford a dark red powder (37.7 g, 88%).
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-24c840048e664bd5a56761d42d4b423b |
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| 出典メモ | uspto-grants-1993_09 |
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