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N,N'-Dimethylurea → 6-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N'-Dimethylurea | HCID 7293 | — |
| 反応物 | Ethyl 3-oxo-3-(pyridin-3-yl)propanoate | HCID 222197 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione | HCID 14096468 | 35.2% |
反応手順
To a mixture of ethyl nicotinoylacetate (2.30 g) and N,N'-dimethylurea (1.05 g) were added conc. hydrochloric acid (a few drops) and ethanol (1 ml) and the mixture was stirred at 110°-115° C. for 4 hours under reduced pressure (30 mmHg). After being cooled to ambient temperature, the solution was adjusted to pH 7.0 with an aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and evaporated to give 6-(3-pyridyl)-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione (0.91 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04612376 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-f9b5bfc73ccf429d972dda2f5938f576 |
| 出典メモ | uspto-grants-1986_09 |