関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-benzyl-6-chloro-1H-pyrimidine-2,4-dione | HCID 937941 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-benzyl-6-chloro-1-(3-chloropropyl)pyrimidine-2,4(1H,3H)-dione | HCID 15027531 | — |
反応手順
To a suspension of 18.93 g (80 mmol) of 3-benzyl-6-chloropyrimidine-2,4(1H,3H)-dione and 17.69 g (128 mmol) of potassium carbonate in 120 ml of N,N-dimethylformamide, 15.8 ml (160 mmol) of 1-bromo-3-chloropropane was added at room temperature. This mixture was stirred at 90° C. for 3 hours. After cooling, the reaction mixture was concentrated to dryness; the resulting residue was dissolved in chloroform-water. After the organic layer was washed with water and dried, the solvent was distilled off to yield an oily substance, which was then purified by column chromatography (eluent, n-hexane/ethyl acetate=5/1→3/1) to yield 13.46 g (53.7%, light yellow powder) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05840732 |
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| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-6d44e8c1a720436b87fa48b2917bc808 |
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| 出典メモ | uspto-grants-1998_11 |
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