関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Bromo-3,5-dimethyladamantane | HCID 98317 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Octane | HCID 356 | — |
| 生成物 | 3,3',5,5'-Tetramethyl-1,1'-biadamantane | HCID 23596970 | 159.6% |
反応手順
A four-neck 1000 ml flask provided with a thermometer, stirrer, and reflux tube was charged with metal sodium 14 g (0.6 mol) and n-octane 600 ml and was cooled to an inside temperature of 0° C. While vigorously stirring, 1-bromo-3,5-dimethyl adamantane 73.0 g (0.3 mol) previously dissolved in n-octane 300 ml was gradually added dropwise. While dropping, the inside temperature was kept at 0° C. to 5° C. After the end of the dropwise addition, when the temperature no longer rose, the reaction was continued for 1 hour. After that, the reactant was poured into cold water 1500 ml, then the crude product was separated by filtration, rinsed with pure water, and dried. Further, the crude product was recrystallized by hot hexane. The obtained recrystallized product was dried under reduced pressure to obtain the product 78.2 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530596B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-29504958b2a54a12b5bf7be1d21503ea |
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| 出典メモ | uspto-grants-2013_09 |
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