참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | 5-(2,6-Dichloro-4-trifluoromethylphenyl)-2-methylbenzenesulfonyl chloride | HCID 22170943 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 1,1'-Thiodi-[5-(2,6-dichloro-4-trifluoromethylphenyl)-2-methylbenzene] | HCID 22170944 | 75% |
반응 단계
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 (nD20 1.6066), which was used in Example 2 (1) as the starting material.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07767626B2 |
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| 출처 데이터셋 | uspto-grants-2010_08 |
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| ORD ID | ord-2239655c1eed4c999c47691f86d14d42 |
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| 출처 메모 | uspto-grants-2010_08 |
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