関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Neophyl chloride | HCID 68191 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | beta-Phenylisovaleric acid | HCID 13890 | 81% |
反応手順
Following a literature procedure, (Leffler, J. E.; Barbas, J. T. JACS. 1981, 103(26), 7768-7773), to a mixture of magnesium turnings (9.5 g) and neophyl chloride (7.5 mL) in tetrahydrofuran (100 mL) is added a spatula tip of iodine and 1,2-dibromoethane (1 mL). The mixture is heated gently with under a heat gun to initiate a vigorous reaction. A solution of neophyl chloride (57 mL) in tetrahydrofuran (360 mL) is added dropwise over the course of 90 minutes. Following completion of the addition, the reaction mixture is stirred for an additional five hours, then solid carbon dioxide (25 g) is added to the flask. After 10 minutes, the flask is transferred to a 40° C. water bath until all carbon dioxide had sublimed. The solvent is then removed under reduced pressure to afford the title compound (58 g, 81%) as a white paste. MS (ES+): (M+H)=178.8
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07390910B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-83009e25d2724ee08cd2ee2fd96be188 |
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| 出典メモ | uspto-grants-2008_06 |
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