関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine hydrochloride | HCID 11130 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 4-Amino-2-chloropyrimidine-5-carbonitrile | HCID 2801166 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Chloro-5-(1H-tetrazol-5-yl)pyrimidin-4-amine | HCID 178508453 | 43.1% |
反応手順
Into a sealed tube were added 4-amino-2-chloro-pyrimidine-5-carbonitrile (837 mg, 5.4 mmol), sodium azide (7.1 mmol, 1.3 eq.), triethylamine hydrochloride (7.1 mmol, 1.3 eq.) and 14 mL of toluene. The tube was tightly capped and the reaction was stirred and heated to 100° C. overnight. The mixture was cooled to room temperature, diluted with ethyl acetate, transferred to a separatory funnel and extracted three times with water. The aqueous extractions were combined and acidified to a pH of 4 with concentrated HCl. The precipitate was collected by filtration, washed with acetonitrile, and dried under vacuum to afford 460 mg of the product, which was used without further purification. MS (EI) for C5HClN7: 198 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08053454B2 |
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| 出典データセット | uspto-grants-2011_11 |
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| ORD ID | ord-68c24091559e4105b47871d18043d828 |
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| 出典メモ | uspto-grants-2011_11 |
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