関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl 3-(trifluoromethyl)benzoate | HCID 520213 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | HCID 178513185 | HCID 178513185 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 178509137 | HCID 178509137 | 13.4% |
反応手順
To a solution of sodium methanolate (1.05 g, 19.44 mmol, 4.00 equiv) in methanol (40 mL) at 0° C. was added aminoguanidine bicarbonate (2.66 g, 19.54 mmol, 4.00 equiv) in several batches. To this was added dropwise a solution of methyl 3-(trifluoromethyl)benzoate (1 g, 4.90 mmol, 1.00 equiv) in methanol (10 mL) with stirring at 0° C. The resulting solution was then stirred overnight at 75° C. in an oil bath. The reaction was then quenched with 10 mL of water/ice, the solution adjusted to pH 3-4 with hydrochloric acid (1 mol/L), and the solids were collected by filtration To afford 150 mg (13%) of 5-(3-(trifluoromethyl)phenyl)-4H-1,2,4-triazol-3-amine as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09289430B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-4e84342d5852438c92fc22a6dfa25169 |
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| 出典メモ | uspto-grants-2016_03 |
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