関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Bromo-9H-fluorene | HCID 14336 | — |
| 反応物 | Orthoperiodic acid | HCID 25289 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-7-iodo-9H-fluorene | HCID 14290982 | 333.6% |
反応手順
Charged were 2-bromofluorene 25.0 g, iodine 11.5 g, orthoperiodic acid 4.88 g, acetic acid 150 ml, conc. sulfuric acid 3 ml and water 10 ml, and the mixture was heated at 60° C. for 30 minutes while stirring. Further, the temperature was elevated up to 90° C., and the mixture was heated for 3 hours while stirring. The reaction solution was left cooling down to room temperature and poured into 500 ml of water. The precipitate formed was filtered and washed with ethanol and water. The solid matter thus obtained was recrystallized from ethanol to obtain 26.5 g of yellow crystal of 2-bromo-7-iodofluorene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425654B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-9f1019e9f08e4c20928a76146f953959 |
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| 出典メモ | uspto-grants-2008_09 |
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