関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,2-Dichloro-4-nitrobenzene | HCID 7443 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3-Fluorobenzylic alcohol | HCID 68008 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Chloro-1-(3-fluoro-benzyloxy)-4-nitro-benzene | HCID 7059269 | 63% |
反応手順
To a mixture of 3-fluorobenzyl alcohol (7.88 g, 62.5 mmol), Aliquot 336 (8.08 g, 20.0 mmol), potassium hydroxide (3.51 g, 62.5 mmol) and water (40 mL) were added toluene (80 mL) and 1,2-dichloro-4-nitrobenzene (10.0 g, 52.1 mmol). The mixture was heated to 60° C. overnight with vigorous stirring. The mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo. The residue was triturated with hot petroleum ether and tert-butyl methyl ether to yield 9.20 g (63%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524722B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-69410e23ead34d7c983e71982da85b2a |
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| 出典メモ | uspto-grants-2013_09 |
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