関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Ethyl-N-benzylaniline | HCID 7098 | — |
| 反応物 | 2,4,4,6-Tetrabromocyclohexa-2,5-dienone | HCID 88433 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-benzyl-N-(4-bromophenyl)-N-ethylamine | HCID 22347350 | 76.6% |
反応手順
N-benzyl-N-phenyl-N-ethylamine (2.25 g, 0.0107 mol) was dissolved in anhydrous dichloromethane (80 mL) and 2,4,4,6-tetrabromocyclohexadiene-1-one (4.36 g, 0.0107 mol) was added in 6 equal portions over a 20 min. period. Stirring was continued at ambient temperature for 20 hours; the organic phase was successively washed with 0.5N solution of sodium hydroxide in water (50 mL), 1N solution of sodium hydroxide in water (50 mL), water (70 mL) and brine (75 mL). The organic phase was dried with magnesium sulfate and concentrated under reduced pressure. The residue was purified by flash chromatography on silica using ethyl acetate/n-heptane (1:99) as mobile phase to yield N-benzyl-N-(4-bromophenyl)-N-ethylamine (2.38 g, 0.0082 mol) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06660744B1 |
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| 出典データセット | uspto-grants-2003_12 |
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| ORD ID | ord-accf4bcf582142b2b40bfe74ca528ad4 |
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| 出典メモ | uspto-grants-2003_12 |
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