関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Propanethiol | HCID 6364 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Chloro-5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrobenzene | HCID 22170938 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | [5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-nitrophenyl]isopropyl sulfide | HCID 22170887 | 90.3% |
反応手順
0.33 g (8.3 mmol) of 60% sodium hydride was stirred in 50 ml of N,N-dimethylformamide at room temperature while 0.7 g (9.2 mmol) of isopropyl mercaptan was added dropwise. After generation of hydrogen was over, 3.0 g (8.1 mmol) of 1-chloro-5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrobenzene was added, and the reaction mixture was stirred at room temperature for 12 hours. The reaction mixture was poured into about 200 ml of ice-cold water and extracted with 50 ml of ethyl acetate twice. The ethyl acetate was washed with 100 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 3.0 g of [5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrophenyl]isopropyl sulfide (yield 90.0%) as a yellow dough (nD20 1.5881).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858639B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-6635c799817e43d0a5b43c7fae22f8d0 |
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| 出典メモ | uspto-grants-2005_02 |
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