関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | 1,4-Bis(trifluoromethyl)benzene | HCID 67945 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 1-Nitro-2,5-bis(trifluoromethyl)benzene | HCID 2734048 | 27.1% |
反応手順
1,4-Bis(trifluoromethyl)benzene (10.06 g, 47 mmol) in fuming sulfuric acid (20 g) was cooled to 0° C. Fuming nitric acid (8 g) was added cautiously. The mixture was heated to 100° C. and stirred for 1 hour. A mixture of fuming nitric acid (6 g) and fuming sulfuric acid (12 g) was added, and the mixture was heated to 110° C. and stirred for 6 hours. After cooling to r.t., the mixture was poured into ice water (150 g) cautiously, and extracted with chloroform (100 mL×3). The combined organic layers were washed with water (100 mL×2), 10% sodium hydroxide aqueous solution (100 mL×2), and then water (100 mL×2). The resulting organic layers were dried over sodium sulfate, filtered, and concentrated to afford 2-nitro-1,4-bis(trifluoromethyl)benzene as an oil (3.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08969349B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-891db7f645a64b44aeffa64ae7ae52b7 |
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| 出典メモ | uspto-grants-2015_03 |
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