関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Furan, 2-(bromomethyl)tetrahydro- | HCID 14501 | — |
| 反応物 | 4-Chlorophenylboronic acid | HCID 74299 | — |
| 反応物 | 2-Aminocyclohexanol hydrochloride | HCID 21877202 | — |
| 反応物 | Sodium hexamethyidisilazane | HCID 45051731 | — |
| 触媒 | Nickel(II) iodide | HCID 26038 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 2-(4-Chloro-benzyl)-tetrahydrofuran | HCID 11644089 | — |
反応手順
To a stirred mixture of (4-chlorophenyl)dihydroxyborane (524.0 mg, 3.351 mmol), 2-aminocyclohexanol hydrochloride (42 mg, 0.28 mmol) and nickel iodide (87.3 mg, 0.279 mmol) in i-PrOH (10.00 mL) was added sodium hexamethyldisilazane (1.075 g, 5.864 mmol) at 0° C. Then the mixture was stirred at rt for 5 min before 2-bromomethyl-tetrahydro-furan (460.00 mg, 2.80 mmol) was added by syringe. The resulting mixture was then stirred at 60° C. for 5 h. The solvent was then removed under reduced pressure and the resulting residue was purified by a flash chromatography(5% AcOEt in hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08481733B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-8671103c7cc1408b9ba4f571600f3510 |
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| 出典メモ | uspto-grants-2013_07 |
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