関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Pempidine | HCID 6603 | — |
| 反応物 | 1,3-dimethyl-1H-pyrazol-4-amine | HCID 4431056 | — |
| 反応物 | 6-Bromo-4-chloro-3-nitroquinoline | HCID 21984128 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | (6-Bromo-3-nitro-quinolin-4-yl)-(1,3-dimethyl-1H-pyrazol-4-yl)-amine | HCID 59619997 | — |
反応手順
To a mixture of 6-bromo-4-chloro-3-nitro-quinoline (Stage A.4, 3.0 g, 20.43 mmol) and 4-amino-1,3-dimethylpyrazole.HCl (ChemCollect, Remscheid, Germany, 1.85 g, 12.53 mmol) in DMA (45 ml) was added 1,2,2,6,6-pentamethylpiperidine (6.67 ml, 36.5 mmol). The RM was stirred at 50° C. for 4.5 h. Then the RM was cooled down to rt and quenched with H2O. The suspension was filtered, the solid cake was washed with H2O and dried under vacuum, before being dissolved in EtOAc. The solution was washed with brine (2×), dried over Na2SO4, filtered and evaporated to dryness to give the title compound as an orange solid (HPLC tR 2.55 min (Method A); M+H=362; M−H=360 MS-ES)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476294B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-107e0d394ec241819ab4fdd628a3d338 |
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| 出典メモ | uspto-grants-2013_07 |
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