関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Homoallyl bromide | HCID 21241 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 1-Bromobut-1-ene | HCID 35945 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 触媒 | 1,1-Dibromoethane | HCID 11201 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178448195 | HCID 178448195 | — |
反応手順
A mixture of magnesium turnings (0.5 g, 0.02 mole) and dry THF (5 mL) were placed in a dry, three-necked round-bottomed flask under argon. To this was added dropwise a solution of 2.3 g (0.7 mole) of 4-bromobutene in 5 mL of dry THF. After about 1/3 of the bromobutene was added, the reaction had not initiated. Two drops of dibromoethane was added and the reaction heated to reflux until Grignard formation was initiated. Heating was stopped and the remainder of the halide was added dropwise to maintain a gentle reflux. After all of the halide was added, the reaction was heated briefly then treated with 1.5 g (0.017 mole) of dioxane with stirring. An immediate white precipitate was formed. This suspension was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04772755 |
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| 出典データセット | uspto-grants-1988_09 |
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| ORD ID | ord-4be068d7828742fc8009d0367e22ccd0 |
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| 出典メモ | uspto-grants-1988_09 |
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