関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Xanthone | HCID 7020 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Potassium tetrafluoroborate | HCID 518872 | — |
| 反応物 | Iodo benzene diacetate | HCID 12217721 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | HCID 23054225 | HCID 23054225 | 47% |
反応手順
To 80 ml of acetic anhydride were suspended 9.8 g (0.05 mol) of xanthene-9-one and 16.1 g (0.05 mol) of iodobenzene diacetate, and 10 g (0.1 mol) of concentrated sulfuric acid was added dropwise thereto at 0 to 7° C. for 1 hour, followed by gradually warming to room temperature and reacting with stirring for 8 hours. After completion of the reaction, the obtained reaction solution was poured into 200 ml of ice water, and 150 ml of toluene was added thereto to dissolve insoluble substance. The solution was fractionated and 12.6 g (0.1 mol) of potassium tetrafluoroborate was added to the obtained water layer, followed by stirring at room temperature for 2 hours. The precipitated crystal was filtered off and dried at 50° C. under vacuum for 2 hours to obtain 11.4 g of 2-(phenyliodonio)xanthene-9-one tetrafluoroborate as pale orange crystal (yield: 47%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07318991B2 |
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| 出典データセット | uspto-grants-2008_01 |
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| ORD ID | ord-8ca9477e10174bbb8db7a98271ad635c |
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| 出典メモ | uspto-grants-2008_01 |
|---|