関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Benzyl-4-chlorophthalazine | HCID 6404566 | — |
| 反応物 | 4-(4-Nitrophenyl)piperidine | HCID 15925817 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | 1-Benzyl-4-[4-(4-nitro-phenyl)-piperidine-1-yl]-phthalazine | HCID 59240568 | 81.6% |
反応手順
To a solution of 1-benzyl-4-chloro-phthalazine (1.08 g, 4.04 mmol) in 8 mL NMP is added 4-(4-nitro-phenyl)piperidine (1 g, 4.85 mmol), TEA (1.68 mL, 12.12 mmol). The reaction mixture was heated to 150° C. for 45 min in a microwave reactor. Water was added to the reaction mixture to form a precipitate and the solid is collected by filtration and dried under vacuum. The resulting solid is purified by HPLC with acetonitril in water (from 20% to 100% with 3% 1-propanol) at 220 nm wavelength detection to provide the title compound (1.4 g, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536168B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-74ca62b13cd84576afb3e3deb18b2930 |
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| 出典メモ | uspto-grants-2013_09 |
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