関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | HCID 178508969 | HCID 178508969 | — |
| 生成物 | 4-Chloro-6-(pyridin-4-yl)pyrimidin-2-amine | HCID 22324286 | — |
反応手順
32 g (170.04 mmol) of the compound (from example XXVIII) are dissolved in 87.1 ml (0.93 mmol) of phosphoryl chloride. 2.80 ml (22.11 mmol) of N,N-dimethylaniline are slowly added dropwise, and the mixture is stirred at 100° C. for one hour. The reaction solution is then stirred at room temperature for another two hours. The phosphoryl chloride is removed under reduced pressure using a rotary evaporator. Water/dichloromethane 9:1 is added to the residue, which is then boiled for 5 minutes. The mixture is then neutralized using saturated sodium bicarbonate solution and the product is filtered off with suction and dried under high vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07737153B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-ed8e5fe2b94d43c7a773afc10623e42a |
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| 出典メモ | uspto-grants-2010_06 |
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