関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 4-Chloro-3-(trifluoromethyl)phenol | HCID 80520 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Chloro-2-nitro-3-(trifluoromethyl)phenol | HCID 58148239 | — |
| 生成物 | 4-Chloro-2-nitro-5-(trifluoromethyl)phenol | HCID 66879688 | — |
反応手順
To a mixture of 5.0 g of 4-chloro-3-trifluoromethylphenol and 20 ml of acetic acid, 1.5 ml of concentrated sulfuric acid and then 2.6 g of 69% nitric acid were added dropwise while ice-cooling. To the reaction mixture, 3 ml of concentrated sulfuric acid was added dropwise at room temperature, and stirred for three hours. The reaction mixture was poured into ice water, and extracted with ethyl acetate. The combined organic layers were washed with water, a saturated aqueous solution of sodium hydrogencarbonate and a saturated sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 2.3 g of 4-chloro-2-nitro-5-trifluoromethylphenol, 1.57 g of 4-chloro-2-nitro-3-trifluoromethylphenol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08242133B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-7ef51ed9cfea4b25884e45e9d1c1b28c |
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| 出典メモ | uspto-grants-2012_08 |
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