関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 2-(Benzofuran-3-yl)ethanol | HCID 10953836 | — |
| 反応物 | Triphenylphosphane dibromide | HCID 12890784 | — |
| 溶媒 | Cyclohexane | HCID 8078 | — |
| 生成物 | 3-(2-bromoethyl)Benzofuran | HCID 15075480 | 83.8% |
反応手順
Triphenylphosphane dibromide (5.52 g, 14.4 mmoles) was suspended in abs. acetonitrile (15 ml) under argon, the suspension was brought to 19° C. in a water-bath and 2-(benzofuran-3-yl)ethanol (2.11 g, 13.1 mmoles) in abs. acetonitrile (7 ml) was added in the course of 15 min. During the addition the temperature of the reaction mixture was kept between 19 and 21° C. The mixture was then left to stand for 12 hours without further cooling. The reaction mixture was filtered and the filtrate obtained was concentrated. The residue obtained was taken up in cyclohexane (20 ml), and the mixture was filtered over a silica gel layer (15 g) about 3 cm thick. The silica gel was washed with cyclohexane (5×20 ml) and the filtrate obtained was concentrated. 2.47 g 3-(2-bromoethyl)benzofuran were obtained as a yellowish oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07951948B2 |
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| 出典データセット | uspto-grants-2011_05 |
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| ORD ID | ord-f518eaf3333d4209b8d56185110bbe4a |
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| 出典メモ | uspto-grants-2011_05 |
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