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Tributylstannane → 1-Fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | 1-Fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene | HCID 53860513 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 1-Fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene | HCID 67632345 | — |
反応手順
Under a nitrogen atmosphere, a stirring solution of 22.7 grams (0.067 mole) of 1-fluoro-1-phenylsulfonyl-3-methyl-3-(4-chlorophenyl)-1-butene, 42.0 grams (0.14 mole) of tributyltin hydride, and 0.5 gram (catalyst) of azobisisobutyronitrile in 700 mL of cyclohexane is heated at reflux for about three hours. After this time the reaction mixture is cooled to ambient temperature, and 125 mL of silica gel is added. The mixture is concentrated under reduced pressure, and the residue is subjected to column chromatography. The product-containing fractions are combined and concentrated under reduced pressure, yielding 1-fluoro-3-(4-chlorophenyl)-3-methyl-1-tributylstannyl-1-butene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05622954 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-beee978054c2486f921e37cce4ee1d7b |
| 出典メモ | uspto-grants-1997_04 |