참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Chlorotrimethylsilane | HCID 6397 | — |
| 반응물 | 3,5-Dibromo-1-trimethylsilylbenzene | HCID 626244 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | (5-Bromo-1,3-phenylene)bis(trimethylsilane) | HCID 12884904 | 94% |
반응 단계
17.18 g of 3,5-Dibromo-trimethylsilyl-benzene, 55.8 mmol, was dissolved in 380 ml Et2O. The solution was chilled to −68° C., and 22.3 mL of n-BuLi (2.5 M in hexanes), 55.8 mmol, were added within 18 minutes. The solution changed its color from clear to yellow, and was stirred for 45 minutes at −68° C. 7.5 mL TMSCl, 59 mmol, were added within six minutes. The temperature of solution rose within one hour to −33° C., and after another 30 minutes to −18° C. The solution was stirred overnight at room temperature. 60 mL of 2M HCl were added to the white suspension. Stirring for 30 minutes resulted in two clear phases. Et2O—phase was dried with MgSO4, filtered, and solvent evaporated. Raw product was distilled at a temperature of 70-76° C. and 0.1-0.2 mbar. All pure fractions were combined and gave 15.8 g of product (52.4 mmol, 94%). 1H-NMR (CHCl3=7.24 ppm): δ 7.56 (s, 2H), 7.50 (t, 1H), 0.25 (s, 6×3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06376409B1 |
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| 출처 데이터셋 | uspto-grants-2002_04 |
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| ORD ID | ord-ac451b3e7e7d440da596d8a5d4a7190e |
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| 출처 메모 | uspto-grants-2002_04 |
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