참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-tert-Butyl-4-methylphenol | HCID 17004 | — |
| 반응물 | HCID 178418573 | HCID 178418573 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | HCID 178426895 | HCID 178426895 | — |
반응 단계
In an atmosphere of nitrogen, 3.29 g (20 mmol) of 2-tert-butyl-4-methylphenol was dissolved in 10 ml of diethyl ether and 6.7 ml of methylmagnesium bromide (20 mmol of diethyl ether solution) was added dropwise to this at 0° C. for 5 minutes. After completion of the dropwise addition, the reaction mixture was stirred at 25° C. for 10 minutes, subsequently, the diethyl ether was evaporated under vacuum, and 30 ml of toluene was added to-obtain a toluene solution of 2-tert-butyl-4-methylphenoxymagnesium bromide. To the solution, 1.07 g (10 mmol) of picolinaldehyde was added dropwise at 25° C. and it was reacted for 5 hours while refluxing. After cooling, the reaction was stopped by adding aqueous 5% hydrochloric acid solution and successively, after neutralizing it with aqueous sodium hydrogencarbonate solution, the organic layer obtained was washed with a saturated aqueous sodium chloride solution. After drying it over anhydrous magnesium sulfate, the solvent was distilled off. The residue was purified by silica gel column chromatography (a developing solvent: hexane/ethyl acetate=20/1-1/1) to obtain 2-bis(2-hydroxy-3-tert-butyl-5-methylphenyl)methylpyridine.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05840646 |
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| 출처 데이터셋 | uspto-grants-1998_11 |
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| ORD ID | ord-fa8039eb9b6249ee858941d40643aea2 |
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| 출처 메모 | uspto-grants-1998_11 |
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