참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium sulfate decahydrate | HCID 62649 | — |
| 반응물 | Methyl 5-(5-methyl-2-phenyl-4-oxazolyl)methoxy-3-pyridinecarboxylate | HCID 17861341 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-(5-Methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridylmethanol | HCID 17861225 | 91.3% |
반응 단계
To a mixture of methyl 5-(5-methyl-2-phenyl-4-oxazolyl)methoxy-3-pyridinecarboxylate (10.70 g) and tetrahydrofuran (100 mL) was added lithium aluminum hydride (1.02 g) under ice-cooling, and the mixture was stirred at room temperature for 10 min. To the mixture was added sodium sulfate 10 hydrate (8.38 g), and the mixture was further stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated. The obtained residue was subjected to silica gel column chromatography to give crystals (8.93 g, 91%) of [5-(5-methyl-2-phenyl-4-oxazolylmethoxy)-3-pyridyl]methanol from a fraction eluted with ethyl acetate-hexane (1:1, v/v). Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 111-112° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07238716B2 |
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| 출처 데이터셋 | uspto-grants-2007_07 |
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| ORD ID | ord-e48f5f9b9def4d44bb3e011585caa42f |
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| 출처 메모 | uspto-grants-2007_07 |
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