참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Methoxy-4-Methylphenol | HCID 7144 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Dimethoxy di-p-cresol | HCID 166971 | 60.5% |
반응 단계
Bu3MeNMnO4 (10.9 g, 34.1 mmol) was dissolved in CH2Cl2 (250 mL) placed in an ice bath and allowed to cool. Then 2-methoxy-4-methylphenol (9.95 g, 72.0 mmol) was added dropwise to the CH2Cl2 solution and allowed to react with stirring for 1 h at 0° C. under N2. The reaction mixture was diluted with H2O (˜200 mL) and the mixture stirred for an additional 30 min. The mixture was filtered through a glass-wool plug to remove the MnO2 and the organic layer separated. The organic layer was washed with 0.1 M HCl (3×150 mL), brine (50 mL), and then dried over MgSO4. Removal of the solvent under reduced pressure afforded 1 as a yellow powder (5.97 g, 60% yield). Purification of 1 was achieved using column chromatography on silica gel and elution with ethyl acetate/hexanes (1/4, v/v) to afford a 50% overall yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09353219B1 |
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| 출처 데이터셋 | uspto-grants-2016_05 |
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| ORD ID | ord-29974e64efcc44118163c0d6c57bb8bc |
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| 출처 메모 | uspto-grants-2016_05 |
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