関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Chloro-N,N-2-trimethylpropenylamine | HCID 640792 | — |
| 反応物 | 4-chloro-1-methyl-1H-pyrazole-5-carboxylic acid | HCID 670823 | — |
| 反応物 | 6-(1H-indol-4-yl)-1H-indazol-4-amine | HCID 58268019 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Chloro-N-[6-(1H-indol-4-yl)-1H-indazol-4-yl]-1-methyl-1H-pyrazole-5-carboxamide | HCID 44540981 | 12.4% |
反応手順
A solution of 4-chloro-1-methyl-1H-pyrazole-5-carboxylic acid (available from Fluorochem) (50 mg) in dry DCM (10 ml) was treated with 1-chloro-N,N,2-trimethyl-1-propen-1-amine (0.041 ml) (available from Acros) and allowed to stir at 20° C. for 10 min when a solution of 6-(1H-indol-4-yl)-1H-indazol-4-amine (77 mg) and triethylamine (0.043 ml) in DCM (5 ml) was added and the mixture stirred at 20° C. for 18 h. The mixture was poured onto an aminopropyl SPE cartridge (1 g) and allowed to stand for 2 h, then the mixture was eluted with methanol (5 ml) and blown to dryness under a stream of nitrogen. The crude product was purified by mass directed preparative HPLC (Method A) to give the title compound as a white solid (15 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08658635B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-2b1ae7de5fd848489294a21c25a2a9c3 |
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| 出典メモ | uspto-grants-2014_02 |
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