関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride | HCID 22170943 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1,1'-Thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene] | HCID 22170944 | 75% |
反応手順
To 0.7 g (18.4 mmol) of lithium aluminum hydride in 30 ml of diethyl ether, 7.2 g (17.8 mmol) of 5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride in 30 ml of diethyl ether was added dropwise at −10° C. After 12 hours of stirring at room temperature, the reaction mixture was poured into 1N aqueous hydrochloric acid for separation. The organic layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography affored 4.3 g of 1,1′-thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene] (yield 75.0%) as a pale yellow dough (nD 1.6066), which was used in Example 2 (1) as the starting material.
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-dbfed1e6ca594ad0befaeb5273844936 |
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| 出典メモ | uspto-grants-2005_02 |
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