関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Chloro-6-hydrazinylpyrimidine | HCID 247222 | — |
| 反応物 | 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68704864 | — |
| 生成物 | HCID 178515349 | HCID 178515349 | — |
反応手順
For 16 h, 2.8 g (19.6 mmol) of the compound from Example 7A and 4.3 g (19.6 mmol) of the compound from Example 3A are stirred in 50 ml of glacial acetic acid at boiling point (bath temperature 125° C.). For work-up, the resulting precipitate is filtered off, the filter residue is washed with diethyl ether and the filtrate is concentrated on a rotary evaporator. The filter residue is dissolved in 50 ml of ethanol, 18.5 ml (2.7 g, 39.2 mmol) of 21% strength ethanolic sodium methoxide solution are added and the solution is stirred at RT for 16 h. The reaction mixture is then adjusted to pH 5 using 1 N hydrochloric acid and stirred at RT for 2 h, the precipitate is then filtered off, the filter residue is washed with water and ethanol and the product is dried under reduced pressure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524699B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-9ca9be7b4b844636ba5b04cd221d2e6d |
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| 出典メモ | uspto-grants-2013_09 |
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