関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromo-1-fluoro-4-nitrobenzene | HCID 69699 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Bromo-1-methylsulfanyl-4-nitrobenzene | HCID 59550842 | — |
反応手順
A solution of 25.7 g (120 mmol) 2-bromo-1-fluoro-4-nitrobenzene in 154 ml DMF is treated with 10.6 g (150 mmol) sodium thiomethylate and stirred for 5 hours at 60° C. The mixture is stirred at room temperature for 18 hours, again treated with 1.0 g sodium thiomethylate and stirred for a further 6 hours at 60° C. After cooling, the mixture is poured into ice-water and extracted with ethyl acetate (3×). The combined organic phases are washed with water, dried (Na2SO4), filtered and concentrated. The residue obtained is chromatographically purified (hexane/ethyl acetate 2:1). 20.4 g (82 mmol, corresponding to 70% of theor.) of the product is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524724B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ba4198057e124a7d9fb4280a99667f3b |
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| 出典メモ | uspto-grants-2013_09 |
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