関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Nitrate | HCID 24434 | — |
| 反応物 | Benzoic acid, 3-fluoro-, methyl ester | HCID 521184 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 5-Fluoro-2-nitrobenzoic acid methyl ester | HCID 5152049 | 96.8% |
反応手順
To a 500 ml, 4-necked flask fitted with a stirrer, thermometer, addition funnel and reflux condenser is charged sulfuric acid (50 ml) and methyl m-fluorobenzoate (8.5 g, 0.055 mole). The reaction mixture is then cooled to 5° C. and a solution of potassium nitrate (reagent 5.57 g, 0.055 mole) is concentrated sulfuric acid (50 ml) is added dropwise over a 30 minute period. Ten minutes after completion of addition the reaction mixture is poured onto 500 g of cracked ice and the product extracted into benzene (3×100 ml). The combined benzene extracts are dried with anhydrous magnesium sulfate and the filtrate reduced in vacuo to give 10.6 g (96%) of product, which is a yellow liquid. Anal. Calcd. for C8H6FNO4 : C, 48.20; H, 3.04; F, 9.54; N, 7.02. Found: C, 50.15; H, 3.34; F, 9.17; N, 6.77.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04259510 |
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| 出典データセット | uspto-grants-1981_03 |
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| ORD ID | ord-aa93bd0cfaa14705a464f6e0293cb454 |
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| 出典メモ | uspto-grants-1981_03 |
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