참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2,6-Diethyl-4-methylphenylacetyl chloride | HCID 57437320 | — |
| 반응물 | Ethyl 2-(methylhydrazono)propanoate | HCID 73828661 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | Ethyl 2-[2-(2,6-diethyl-4-methylphenylacetyl)-2-methylhydrazono]propanoate | HCID 76550641 | 49.4% |
반응 단계
1.5 g of potassium carbonate was added to a solution of 2.0 g of ethyl 2-(methylhydrazono)propanoate in 35 mL of acetonitrile. The mixture was stirred under cooling with ice, to which a solution of 2.6 g of 2,6-diethyl-4-methylphenylacetyl chloride in 10 mL of acetonitrile was added dropwise over about 20 minutes. The resulting mixture was further stirred for 3.5 hours at room temperature, and then concentrated under reduced pressure. To the residue obtained was added 20 mL of ice-water, which was extracted with ethyl acetate (20 mL×3). The extracts were combined, washed with a saturated sodium chloride aqueous solution (20 mL×2), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was subjected to basic alumina column chromatography (ethyl acetate:hexane=1:3 as eluent) to yield 1.9 g of the title compound as white crystals.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541414B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-386370daeb3c4bb9a6c03a4cd0dabdc2 |
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| 출처 메모 | uspto-grants-2013_09 |
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