関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tin tetrachloride | HCID 24287 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-(2,5-Dichloro-phenoxy)-2-fluoro-4-nitro-benzene | HCID 59798046 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(2,5-Dichlorophenoxy)-3-fluoroaniline | HCID 28972706 | — |
反応手順
A mixture of 1-(2,5-dichloro-phenoxy)-2-fluoro-4-nitro-benzene (0.5 g, 1.7 mmol) and tin chloride (1.57 g, 8.3 mmol) in 30 ml of anhydrous ethanol was heated to 70° C. under argon and stirred for 4 hours. The solution was allowed to cool and then poured into ice. The solution was made slightly basic (pH 7-8) by addition of saturated aqueous sodium bicarbonate solution, then extracted with ethyl acetate. The organic phase was thoroughly washed with brine and dried treated with anhydrous sodium sulfate. Evaporation of the solvent left a yellow oily product which was used for the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07429667B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-3f16de5a631343f9ab6d061ff9289df8 |
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| 出典メモ | uspto-grants-2008_09 |
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