참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Phosphonic acid, [2-(4-morpholinyl)-2-oxoethyl]-, diethyl ester | HCID 11207805 | — |
| 반응물 | HCID 14878846 | HCID 14878846 | — |
| 용매 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 생성물 | HCID 54229760 | HCID 54229760 | 31.7% |
반응 단계
In 1,2-dimethoxyethane (10 ml) was suspended 60% sodium hydride (dispersion in paraffin) (132 mg). To the suspension was added dropwise, while stirring, a solution of diethylphosphonoacetic acid morpholide (688 mg) in 1,2-dimethoxyethane (5 ml). To the mixture was added 2-(2-chlorophenoxy)-5-(3,4-dimethoxybenzoyl)pyridine (800 mg), which was heated for 8 hours under reflux. The reaction mixture was concentrated and the residue was dissolved in ether, washed with water and dried over anhydrous magnesium sulfate. The solvent was then distilled off to leave an oily substance, which was purified by means of a silica gel chromatography (eluted with ethyl acetate) to obtain 4-[3-(2-(2-chlorophenoxy)-5-pyridyl)-3-(3,4-dimethoxyphenyl)acryloyl]morpholine (Compound No.1) (330 mg) as a resinous solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04954497 |
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| 출처 데이터셋 | uspto-grants-1990_09 |
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| ORD ID | ord-b1d6e2d05cab486c9ad94dfadc2dbe51 |
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| 출처 메모 | uspto-grants-1990_09 |
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