関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 4-Fluorobenzylic alcohol | HCID 68022 | — |
| 反応物 | Sodium Bromate | HCID 23668195 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | 4-Fluorobenzoic Acid | HCID 9973 | 86% |
反応手順
A mixture of the Ceiv catalyst from Example 47 (0.08 g), sodium bromate (0.3 g) and 4-fluorobenzyl alcohol (0.256 g, 2 mmol) in acetonitrile:water (1:1, 10 ml) was stirred at 80° C. for 40 h under an atmosphere of nitrogen. On cooling ether (70 ml) was added and the catalyst was filtered off. The organic layer was separated and the aqueous phase was extracted with ether (2×50 ml). The combined organic extracts were washed with water (25 ml), dried with anhydrous magnesium sulphate and concentrated to give 4-fluorobenzoic acid as a white solid (0.24 g, 86%). M.p. 182° C., lit. 185° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728159B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-07562343ab814930ba62f565d02c2dcd |
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| 出典メモ | uspto-grants-2010_06 |
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