참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Quinazolinedione | HCID 64048 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | 4-[(3-Chloropropyl)sulfanyl]pyridine | HCID 15816984 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[3-(4-pyridylthio)propyl]quinazoline-2,4(1H,3H)-dione | HCID 19079092 | 31.1% |
반응 단계
To a solution of 1.62 g (10 mmol) of benzoylene urea and 1.88 g (10 mmol) of 4-(3-chloropropylthio)pyridine in 50 ml of dimethylformamide, 1.65 ml (11 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, and the mixture was stirred at 80° C. for 16 hours. After cooling, water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was dried and the solvent was distilled off. The residue was purified by column chromatography (eluent:ethyl acetate/ethanol=25:1 to 10:1 to 2:1). First, 0.973 g of 3-[3-(4-pyridylthio)propyl]quinazoline-2,4-(1H,3H)-dione (31.1% yield, pale yellow crystals) was obtained, and then, 0.487 g of the desired product was obtained (10.4% yield, yellow oil).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05561147 |
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| 출처 데이터셋 | uspto-grants-1996_10 |
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| ORD ID | ord-23d280a50411417ca88c8e86ccf73a33 |
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| 출처 메모 | uspto-grants-1996_10 |
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