関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Nitro-2,5-bis(trifluoromethyl)benzene | HCID 2734048 | — |
| 反応物 | Tin dichloride dihydrate | HCID 43835034 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,5-Bis(trifluoromethyl)aniline | HCID 719818 | 85.9% |
反応手順
To a solution of 2-nitro-1,4-bis(trifluoromethyl)benzene (3.3 g, 12.7 mmol) in methanol (15 mL) was added a solution of SnCl2.H2O (8.57 g, 38.1 mmol) in conc. HCl (15 mL) at room temperature, and the mixture was heated to 50° C. and stirred for 4 hours. Methanol was removed, and the aqueous solution was basified with conc. NaOH solution until pH 10. The suspension was diluted with EtOAc (100 mL), and the mixture was stirred at room temperature for 30 minutes and filtered. The solid was discarded, and the filtrate was washed with brine (50 mL), dried over sodium sulfate, and filtered. The solution was concentrated to give 2,5-bis(trifluoromethyl)benzenamine as a yellow oil (2.5 g). MS (ESI): m/z 230 [M+H]+.
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-0a858d2e28904dfdb0f31798423e5cef |
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| 出典メモ | uspto-grants-2015_03 |
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