関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Uracil | HCID 1174 | — |
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Nitrophenyl)pyrimidine-2,4-dione | HCID 11276338 | 57.6% |
反応手順
To a stirred solution of 42.8 parts of sodium hydride dispersion 50% in 200 parts of dimethyl sulfoxide was added dropwise slowly a solution of 50 parts of 2,4(1H,3H)-pyrimidinedione in 800 parts of dimethyl sulfoxide while the temperature was kept constant (20° C.) by cooling in an ice/water bath. 62.9 Parts of 1-fluoro-4-nitrobenzene were added and the whole was stirred overnight at 50° C. After cooling, the reaction mixture was poured into 2500 parts of water. The whole was washed with dichloromethane. The aqueous phase was brought to pH 5-6. The product was filtered off and stirred in 2-propanone. The product was filtered off and dried in vacuo at 60° C., yielding 60 parts (57.6%) of 1-(4-nitrophenyl)-2,4(1H,3H)-pyrimidinedione; mp.>300° C. (int. 23).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04931444 |
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| 出典データセット | uspto-grants-1990_06 |
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| ORD ID | ord-c2fcd2a5cac34cc68e16028d5d86afc3 |
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| 出典メモ | uspto-grants-1990_06 |
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