関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3-Hydrazinyl-6-phenylpyridazine | HCID 6409842 | — |
| 反応物 | 2-(Quinolin-6-yl)propanoic acid | HCID 19036006 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 6-(1-(6-Phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)ethyl)quinoline | HCID 57691387 | 54.5% |
反応手順
To a 2-5 ml Personal Chemistry microwave vial was added 2-(quinolin-6-yl)propanoic acid (0.25 g, 1.2 mmol), 1-(6-phenylpyridazin-3-yl)hydrazine (0.42 g, 2.2 mmol) and conc. HCl (2 mL). The mixture was heated in the microwave at 160° C. for 8 h. After cooling to rt, the mixture was poured into sat. NaHCO3 (100 mL) and then extracted with EtOAc (4×75 mL). The combined extracts were washed with brine, dried (Na2SO4) and concentrated onto silica. Purification by silica gel chromatography (1.0 to 4.5% MeOH (2 M in NH3)/CH2Cl2) afforded the title compound as an off-white solid (0.23 g, 53% yield). MS (ESI, pos. ion) m/z: 352 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524900B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-53fcc463ca32451a88043f30d34a083f |
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| 出典メモ | uspto-grants-2013_09 |
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