참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Homoallyl bromide | HCID 21241 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 1-Bromobut-1-ene | HCID 35945 | — |
| 반응물 | Magnesium | HCID 5462224 | — |
| 촉매 | 1,1-Dibromoethane | HCID 11201 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 178448195 | HCID 178448195 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04772755 |
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| 출처 데이터셋 | uspto-grants-1988_09 |
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| ORD ID | ord-4be068d7828742fc8009d0367e22ccd0 |
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| 출처 메모 | uspto-grants-1988_09 |
|---|