참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| 반응물 | N-Benzylaminodiacetic acid | HCID 77606 | — |
| 반응물 | 7-Methoxynaphthalen-1-amine | HCID 235817 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(7-Methoxy-1-naphthyl)-4-benzyl-2,6-piperazinedione | HCID 19808487 | 82% |
반응 단계
126 mmol (2.2 equivalents) of carbonyldiimidazole are added to a suspension containing 58 mmol (1 equivalent) of N-benzyliminodiacetic acid in 200 ml of anhydrous tetrahydrofuran. The mixture is brought to reflux until the evolution of CO2 has ceased. A solution containing 58 mmol (1 equivalent) of 1-amino-7-methoxynaphthalene in 40 ml of anhydrous tetrahydrofuran is then added to the above mixture. The resulting mixture is brought to reflux for 20 hours, the solvent is evaporated off and the residue obtained is taken up with 300 ml of anhydrous ethanol. The precipitate formed is filtered off and then dissolved in 200 ml of dichloromethane. The insoluble matter is filtered off and the filtrate concentrated. The expected product is then obtained after taking up in isopropyl ether followed by filtration.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05166156 |
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| 출처 데이터셋 | uspto-grants-1992_11 |
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| ORD ID | ord-0f62f74f5ae2418196acafa38547bcb3 |
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| 출처 메모 | uspto-grants-1992_11 |
|---|