関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 1-methyl-1H-indazol-6-amine | HCID 840433 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Sulfuric acid hydrate (1:1) | HCID 21910475 | — |
| 生成物 | 1-methyl-1H-indazol-6-ol | HCID 135503223 | — |
反応手順
To a solution of 1-methyl-1H-indazol-6-amine (300 mg, 2.04 mmol) in H2O/H2SO4=1:1 (5 ml) was added NaNO2 (141 mg, 2.04 mmol) at 0° C. The mixture was then stirred for 2 h at 25° C. before being added to water (0.5 ml) and stirred for a further 2 h at 120° C. Once the reaction was complete by TLC, the mixture was treated with NaHCO3 until pH=7. The mixture was then extracted with ethyl acetate (2×10 ml) and the organic layer washed with brine (20 ml), dried over Na2SO4 and concentrated to give 1-methyl-1H-indazol-6-ol as a red solid which was used in the next step without further purification (300 mg, 99.0%). LCMS (m/z):149.1 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09266836B2 |
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| 出典データセット | uspto-grants-2016_02 |
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| ORD ID | ord-112fdb30df964db7a83922749d57d180 |
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| 出典メモ | uspto-grants-2016_02 |
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