참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 2-Naphthalenecarboxaldehyde | HCID 6201 | — |
| 반응물 | 3-Bromo-2-chlorothiophene | HCID 2724559 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | HCID 23070162 | HCID 23070162 | 84.8% |
반응 단계
Under nitrogen atmosphere, to a solution of 3.2 mL of 1.57 M n-butyllithium in hexane in 7 mL of diethyl ether was added a solution of 1.00 g of 3-bromo-2-chlorothiophene in 8 mL diethyl ether at −78° C., and stirred at this temperature for 1 hour. At the same temperature, 0.87 g of 2-naphthaldehyde was added, stirred for 3 hours while raising the temperature to room temperature, then added with water, extracted with ethylacetate, washed successively with saturated aqueous ammonium chloride and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resultant crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:20-1:5), to afford 1.18 g of the title compound as colorless crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07429609B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-4a80a6305a224c85bee56ea956bdbaea |
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| 출처 메모 | uspto-grants-2008_09 |
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