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HRID 273289作成日:2026年10月25日
Benzenamine, 3-bromo-4-methyl- → N-(3-bromo-4-methyl-phenyl)4-(4-methyl-piperazin-1-ylmethyl)-benzamide
https://huagongshe.com/reaction/273289
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenamine, 3-bromo-4-methyl- | HCID 82187 | — |
| 反応物 | Methyl 4-((4-methylpiperazin-1-yl)methyl)benzoate | HCID 782222 | — |
| 反応物 | Trimethylaluminum | HCID 16682925 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-(3-bromo-4-methyl-phenyl)4-(4-methyl-piperazin-1-ylmethyl)-benzamide | HCID 10309714 | — |
反応手順
A solution of trimethylaluminium (2M in toluene, 15.0 ml) is added over a period of 30 min to a solution of 3-bromo-4-methyl-aniline(2.15 g, 11.5 mmol) and 4-(4-methyl-piperazin-1-ylmethyl)-benzoic acid methyl ester (2.87 g, 11.5 mmol) in toluene (20 ml) at 40° C. under an atmosphere of argon. After gas evolution ceases, the reaction mixture is stirred 30 min before being cooled to 0° C. and partitioned between cold aqueous 1N NaOH (100 ml) and toluene (100 ml). The organic layer is extracted with aqueous saturated NH4Cl (100 ml) and aqueous saturated NaCl (100 ml) The organic layer is concentrated in vacuo to give 4.69 g (97 area % by HPLC) of the title compound as pale yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07456283B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-a96d00eed30545c5bcbe3c64f9b42c98 |
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| 出典メモ | uspto-grants-2008_11 |
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