참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Diketene | HCID 12661 | — |
| 반응물 | 2-Propenamide, N-(3-aminopropyl)-2-methyl-, hydrochloride (1:1) | HCID 10375005 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | N-(3-Methacrylamidopropyl)-3-oxobutanamide | HCID 23223314 | 50% |
반응 단계
Triethylamine (24 g, 0.24 mole) was added dropwise at 0° C. to a solution of N-(3-aminopropyl)-methacrylamide hydrochloride (40 g, 0.24 mole) and diketene (20 g, 0.24 mole) in methanol (800 ml). After addition, the temperature was maintained at 0° C. for 2 hours under stirring. Stirring was continued at 20° C. for 20 hours. The solvent was then removed. The residue was dissolved in chloroform (1 liter), washed with 5% hydrochloric acid (200 ml), washed with saturated NaHCO3 (200 ml), dried over anhydrous magnesium sulfate, and filtered. Excess solvent was removed. The residue was recrystallized from benzene (500 ml) and ethyl ether (500 ml) to give N-(3-acetoacetamidopropyl)methacrylamide (m.p.=93°-94° C.) at a yield of 50%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04346231 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-b568e52c429c41d884e4a5fac2e5a3f6 |
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| 출처 메모 | uspto-grants-1982_08 |
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