関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Picolyl chloride | HCID 23393 | — |
| 反応物 | HCID 178507909 | HCID 178507909 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Amino-2-(2-pyridylmethylthio)-pyrimidine | HCID 15550150 | — |
反応手順
4-Amino-2-mercaptopyrimidine (0.40 g, 3.15 mmol) is slurried in ethanol (2 ml) and 3.25 M NaOH (2.0 ml, 6.5 mmol) is added. The solution is heated to reflux for 10 minutes and after cooling to 22° C., 2-picolyl chloride*HCl (0.49 g, 2.98 mmol) is added. The solution is heated to reflux for an additional 15 minutes. The solution is cooled and concentrated in vacuo. The residue is dissolved in 1 N HCl and diluted with ethyl acetate. The mixture is neutralized with NaOH to pH 8 and the aqueous layer is separated and washed twice with ethyl acetate. The combined organic layers are washed with saturated NaHCO3, saturated NaCl, dried with MgSO4 and concentrated in vacuo, mp 133-134° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05981537 |
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| 出典データセット | uspto-grants-1999_11 |
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| ORD ID | ord-c375a34da3aa43aaa543819785b801f3 |
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| 出典メモ | uspto-grants-1999_11 |
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