関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 6-Amino-3-oxo-2,3-dihydro-indazole-1-carboxylic acid tert-butyl ester | HCID 57498019 | — |
| 反応物 | HCID 178478385 | HCID 178478385 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178518850 | HCID 178518850 | 49.9% |
反応手順
To a sealed tube was added (4-Chloro-6-phenyl-[1,3,5]triazin-2-yl)-(5-cyclopropyl-2H-pyrazol-3-yl)-amine (50 mg, 0.16 mmol) and 6-amino-3-oxo-2,3-dihydro-indazole-1-carboxylic acid tert-butyl ester (80 mg, 0.32 mmol) in 1 ml of n-butanol. The contents were heated to 85° C. for 3 hours. The reaction was concentrated in vacuo to give a white solid that was dissolved in 3 ml of dichloromethane and 1 ml of trifluoro acetic acid and stirred for 5 hours at room temperature. The reaction concentrated and the crude residue purified by prep HPLC to afford 34 mg of the desired product as a light yellow solid (39.4% yield). H-NMR (DMSO-d6, 500 mHz) δ 10.95 (m, 1H), 10.30 (m, 1H), 9.91 (s, 1H), 8.32 (m, 2H), 8.04 (m, 1H), 7.49 (m, 4H), 7.25 (m, 1H), 6.14 (s br, 1H), 1.85 (s, 1H), 0.87 (s, 2H), 0.67 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07842712B2 |
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| 出典データセット | uspto-grants-2010_11 |
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| ORD ID | ord-58beefd029bf434e98e6d98b120e4924 |
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| 出典メモ | uspto-grants-2010_11 |
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