関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | (3-Bromophenyl)(phenyl)methanol | HCID 285827 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethoxyethane ethanol | HCID 20074477 | — |
| 溶媒 | Diethyl ether methanol | HCID 21864698 | — |
| 生成物 | 1-Benzyl-3-bromobenzene | HCID 597532 | 71.17% |
反応手順
To a suspension of 422 mg (11.12 mmol, 1.31 eq.) lithium aluminum hydride in 30 ml dry ether a solution of 1.38 g (10.35 mmol, 1.22 eq.) aluminum chloride in 18 ml dry ether was added cautiously under stirring. After the complete addition the resulting mixture was stirred for 30 min at r.t. before a solution of 2.24 g (8.52 mmol) (3-Bromo-phenyl)-phenyl-methanol (prepared above) in 19 ml dry ether was added dropwise. Then the mixture was refluxed for 12 h and after that cooled to 0° C. in an ice-bath. After adding cautiously 10 ml of a mixture of ether/methanol (1:1) 28 ml 1 N HCl-solution was added and the mixture was extracted with ether. The comb. org. fractions were washed with brine, dried over Na2SO4 and evaporated. Column chromatography (PE/CH2Cl2 (9+1)) yielded 1.50 g (6.06 mmol, 71.17%) 1-Benzyl-3-bromo-benzene (87) as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07312246B2 |
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| 出典データセット | uspto-grants-2007_12 |
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| ORD ID | ord-482421c05a11405b9e4accf39b0e8e99 |
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| 出典メモ | uspto-grants-2007_12 |
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