참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Undec-4-ene | HCID 136496 | — |
| 반응물 | Diethyl 2-(3-bromopropionamido)malonate | HCID 19045185 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Diethyl 2-oxopyrrolidine-5,5-dicarboxylate | HCID 19045188 | 37.3% |
반응 단계
2(b) 314 μl of 1,8-diaza[5.4.0]-7-undecene were added to a solution of 620 mg of diethyl 2-(3-bromopropionamido)malonate (prepared as described above) dissolved in methylene chloride, and the mixture was stirred at room temperature for 3 hours. At the end of this time, the reaction mixture was concentrated by evaporation under reduced pressure, poured into water and then extracted with diethyl ether. The extract was washed with 5% w/v aqueous hydrochloric acid, with a 5% w/v aqueous solution of sodium bicarbonate and with water, in that order, and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give a crude product. This was purified by column chromatography through silica gel, eluted with a 2:1 by volume mixture of cyclohexane and ethyl acetate, to give 171 mg of diethyl 2-oxopyrrolidine-5,5-dicarboxylate.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05527905 |
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| 출처 데이터셋 | uspto-grants-1996_06 |
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| ORD ID | ord-5e6e85e2d9d8426d99779a089a22f9f3 |
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| 출처 메모 | uspto-grants-1996_06 |
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