関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | Indazole-3-carboxylic acid | HCID 78250 | — |
| 反応物 | Bis-(1H-imidazol-2-YL)-methanone | HCID 5250894 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N,N-Dimethyl-1H-indazole-3-carboxamide | HCID 20816326 | — |
反応手順
1H-Indazole-3-carboxylic acid (5.0 g, 30.8 mmol) and carbonyl diimidazole (5.0 g, 33.9 mmol) were dissolved in N,N-dimethylformamide (150 mL) and heated to 60° C. After 2 hours, dimethylamine hydrochloride (4.0 g, 33.9) was added, and the reaction was stirred for an additional hour at 60° C. The reaction was poured into water, and the aqueous phase was extracted with ethyl acetate (3×150 mL). The combined organic phases were washed sequentially with aqueous sodium bicarbonate, 10% hydrochloric acid, water and brine. After drying over magnesium sulfate, filtering and concentrating in vacuo, the title compound was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08648069B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-8e15ba4e94764231a73f3a5ba168eef4 |
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| 出典メモ | uspto-grants-2014_02 |
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