関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Quinazolinedione | HCID 64048 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | 2-(4-Chlorobutylthio)pyridine | HCID 19079186 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,3-bis[4-(2-pyridylthio)butyl]quinazoline-2,4(1H,3H)-dione | HCID 19079232 | 9% |
反応手順
To a solution of 1.62 g (10 mmol) of benzoylene urea and 2.02 g (10 mmol) of 2-(4-chlorobutylthio)pyridine in 50 ml of dimethylformamide, 1.65 ml (11mmol) 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:hexane/ethyl acetate=2:1 to 1:2). First, 221 mg of the desired product was obtained (4.6% yield, yellow oil), and then, 292 mg of 3-[4-(2-pyridylthio)butyl]quinazoline-2,4(1H,3H)-dione was obtained (8.9% yield, white crystals).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05561147 |
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| 出典データセット | uspto-grants-1996_10 |
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| ORD ID | ord-9d3f66780e5642d3a4d5c2da31efc980 |
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| 出典メモ | uspto-grants-1996_10 |
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