참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | Tetraethoxysilane | HCID 6517 | — |
| 반응물 | Diisopropylaniline | HCID 32484 | — |
| 반응물 | (3-Bromo-2-hydroxy-5-methylphenyl)(phenyl)methanone | HCID 12925474 | — |
| 생성물 | HCID 178422466 | HCID 178422466 | 69.1% |
반응 단계
In a 50 mL Claisens flask under an argon atmosphere, a mixture of 13.5 g (46.3 mmol) of 33, 20.2 g (97.2 mmol) of Si(OEt)4, and 9.03 g (50.9 mmol) of 2,6-diisopropylaniline was heated to 170° C., and then 0.37 mL of 96% H2SO4 was added. This mixture was stirred at this temperature for 35 hr, and the formed ethanol was slowly distilled off Later, 300 mL of cold water was added, and the product was extracted with 2×100 mL of diethyl ether. The combined extract was dried over K2CO3 and then evaporated to dryness. The product was isolated by flash-chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether, 100:1, vol.). This procedure gave 14.4 g (69%) of 34.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541521B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-56d393942c2e4aacabe825b5238a6eff |
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| 출처 메모 | uspto-grants-2013_09 |
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