関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phloroglucinol | HCID 359 | — |
| 反応物 | 2,3-Dimethoxybenzoic acid | HCID 15204 | — |
| 生成物 | 1,3-dihydroxy-5-methoxy-9H-xanthen-9-one | HCID 12026489 | 94.8% |
反応手順
2,3-dimethoxybenzoic acid (0.91 g, 5 mmol), phloroglucinol (0.95 g, 7.5 mmol), ZnCl□ (4.69 g, 30 mmol) and POCl□ (20 mL) were charged to a dry round-bottom flask, followed by stirring at 80° C. for 4 hours. After the reaction was completed, the reaction mixture was cooled to room temperature and was very slowly added to 500 mL of ice water. When the reaction liquid was poured in ice water, ice was added portionwise to prevent overheating. The resulting precipitate was allowed to stand at 4° C. overnight, combined, washed with water and ether, and then dried under reduced pressure to give the title compound (1.22 g, 94.8%) as a reddish brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846749B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-88281e7637434075ba1a3856a89d84a5 |
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| 出典メモ | uspto-grants-2014_09 |
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