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Methanol → 1-Bromo-4-phenylbutane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Benzenebutanol | HCID 76889 | — |
| 反応物 | Triphenylphosphane dibromide | HCID 12890784 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-Bromo-4-phenylbutane | HCID 259668 | 106.3% |
反応手順
To a solution of 4-phenyl-1-butanol (21.75 g) in acetonitrile (300 mL) was added triphenylphosphine dibromide (67.23 g) in portions with stirring over 10 min. After stirring over night under nitrogen, methanol (4 mL) was added and after 1.5 h, the solvent was removed under reduced pressure. Hexanes (200 mL) and ˜75 g silica gel were added to the residue and the mixture was filtered and the filter cake was eluted with hexanes. The clear filtrate was concentrated to give 32.8 g of clear colorless liquid. This product was again eluted through silica gel using 1.5 L hexanes to give the title compound (24.7 g) as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06358979B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-06693a3616814cb881bb4b289a4578b1 |
| 出典メモ | uspto-grants-2002_03 |