참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | Ethyl (2,6-diethyl-4-methylphenyl)glyoxylate | HCID 56942718 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 2-(2,6-Diethyl-4-methylphenyl)-2-oxoacetohydrazide | HCID 56942873 | 39.8% |
반응 단계
To a 100 ml volume four-necked flask, methanol (22.91 g) and hydrazine hydrate (1.93 g) were added at room temperature, and cooled. Ethyl 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetate (9-a) (5.01 g) diluted with methanol (10.02 g) was added dropwise at 1° C. over 5 minutes. The resulting mixture was stirred at 2° C. for 4 hours, then the mixture was filtered. The resulting filtrate was concentrated, added tert-butyl methyl ether (41 g), and washed with brine (14 g). The resulting organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography (silica gel: 40 g, hexane:ethyl acetate=1:1) to gave 1.88 g of 2-(2,6-diethyl-4-methylphenyl)-2-oxoacetohydrazide ((12-1)-(11)-39).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08884010B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-6a5931a32b8f45f7b72b66bd9ce9b3d1 |
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| 출처 메모 | uspto-grants-2014_11 |
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