関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | 1-Pyrenemethanol | HCID 104977 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(Bromomethyl)pyrene | HCID 1274043 | — |
反応手順
Firstly, 500 mg of (1-pyrenyl)methanol as the starting material was dissolved in 20 mL of dehydrated dichloromethane, and then 1 mL of PBr3 was slowly dropped into the solution that was kept in an ice bath of 0° C. in an N2-atmosphere. After 12 hours of stirring with a magnetic stirrer, the mixture was neutralized with 50 ml of 0.3M sodium bicarbonate solution (4 g/150 mL) three times using a separating funnel, and then CH2Cl2 was used to extract the organic phase in the mixture. After the moisture in the organic phase was removed by anhydrous MgSO4, the solvent in the organic phase was removed under a reduced pressure to obtain 547 mg of (1-pyrenyl)bromomethane in a high purity. The completion of the bromination was confirmed by the 1H-NMR spectrum of the product in FIG. 3A and the mass spectrum (molecular weight=295.17) of the same.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07754107B2 |
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| 出典データセット | uspto-grants-2010_07 |
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| ORD ID | ord-a2d13e8ea58f4d06abef20701b4a8dd8 |
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| 出典メモ | uspto-grants-2010_07 |
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