関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 5-Chloro-3-((trimethylsilyl)ethynyl)pyridin-2-amine | HCID 24729465 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Chloro-3-ethynylpyridin-2-amine | HCID 25918667 | 89.3% |
反応手順
A suspension of 1.6 g of 5-chloro-3-trimethylsilanylethynylpyridin-2-ylamine and 1.24 g of potassium fluoride in 80 ml of methanol is brought to reflux for approximately 3 hours 30 minutes. After returning to a temperature in the region of 20° C., the mixture is filtered through celite, and the insoluble material is washed three times with 50 ml of methanol. The filtrate is concentrated to dryness under reduced pressure (13 kPa). The residue is taken up with 100 ml of dichloromethane. The solution obtained is washed with three times 60 ml of water, dried over magnesium sulfate, filtered, and concentrated to dryness under reduced pressure (13 kPa). 0.97 g of 5-chloro-3-ethynylpyridin-2-ylamine is thus obtained in the form of a solid, the characteristics of which are as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07528147B2 |
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| 出典データセット | uspto-grants-2009_05 |
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| ORD ID | ord-fbb17af726ac46589fe669405f1ad55a |
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| 出典メモ | uspto-grants-2009_05 |
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