関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Amino-5-chloropyridine | HCID 66174 | — |
| 反応物 | N-Iodosuccinimide | HCID 120273 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Amino-5-chloro-3-iodopyridine | HCID 11076010 | 97% |
反応手順
A mixture of 6.43 g of 5-chloropyridin-2-ylamine and 12.38 g of N-iodosuccinimide in 300 ml of glacial acetic acid is heated at around 55° C. for 6 hours. After returning to a temperature of approximately 20° C., the mixture is agitated for approximately 18 hours and then concentrated to dryness under reduced pressure (13 kPa). The residue is taken up with 400 ml of water; the pH of the suspension obtained is brought back to approximately 8 by adding a saturated aqueous sodium hydrogen carbonate solution. The precipitate is filter-dried, washed with water, and dried at 40° C. under reduced pressure (13 kPa) for approximately 3 hours. 12.35 g of 5-chloro-3-iodopyridin-2-ylamine are 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-506e8cb1709847888265fbbfa270d949 |
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| 出典メモ | uspto-grants-2009_05 |
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