関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | (4-Methoxy-2-methylphenyl)boronic acid | HCID 2773486 | — |
| 反応物 | 3-Amino-4-bromo-6-chloropyridazine | HCID 22024419 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-Chloro-4-(4-methoxy-2-methylphenyl)-3-pyridazineamine | HCID 22024474 | 54.9% |
反応手順
4-Bromo-6-chloro-3-pyridazineamine (12 g) and 4-methoxy-2-methylphenylboronic acid (10.5 g) were dissolved in a mixed solvent of toluene (240 mL) and ethanol (45 mL), then tetrakistriphenylphosphine palladium complex (6.7 g) and a 2M aqueous sodium carbonate solution (24 mL) were added thereto, and the mixture was heated under stirring at 100° C. for 12 hours. After completion of the reaction, the solvent was evaporated. The residue was extracted with ethyl acetate, washed with water, and dried over anhydrous magnesium sulfate, and then the solvent was evaporated. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:4) to give the title compound (7.89 g) as brown crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07772249B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-6fa9ab8aece6499dba6053cbaea6e650 |
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| 出典メモ | uspto-grants-2010_08 |
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