참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Diphenyl Ether | HCID 7583 | — |
| 반응물 | Diethyl[(4-quinazolinylamino)methylene]propanedioate | HCID 13060467 | — |
| 용매 | Hexane | HCID 8058 | — |
| 생성물 | ethyl 4-oxo-4H-pyrimido[1,2-c]quinazoline-3-carboxylate | HCID 13060520 | 90.8% |
반응 단계
To diethyl [(4-quinazolinylamino)methylene]propanedioate (16.0 g) was added diphenylether (70 ml) which had been heated at 250° C. in advance. The reaction mixture was stirred at 250°-260° C. for 20 minutes and cooled to ambient temperature. To the resultant mixture was added hexane. The mixture was stirred to give crystals, which was washed with hexane and dried. The crude crystals were dissolved in ethyl acetate under heating. After insoluble materials were removed by filtration, the filtrate was concentrated under reduced pressure to a volume of 200 ml. To the concentrate was added hexane and the mixture was allowed to stand at ambient temperature to precipitate crystals, which were separated by filtration, washed with a mixture of ethyl acetate and hexane and dried to give crystalline ethyl 4-oxo-4H-pyrimido[1,2-c]quinazoline-3-carboxylate (12.4 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04543356 |
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| 출처 데이터셋 | uspto-grants-1985_09 |
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| ORD ID | ord-9c0252119bc2462a8ddcfab6c5a55556 |
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| 출처 메모 | uspto-grants-1985_09 |
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