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Ethylene Glycol → N-Methyl-N-phenylbenzylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | N-Methylbenzylamine | HCID 7669 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Ethyl acetate hexane | HCID 21226206 | — |
| 生成物 | N-Methyl-N-phenylbenzylamine | HCID 69191 | 74% |
反応手順
The general procedure under argon was followed using copper(I) iodide (19 mg, 0.10 mmol), K3PO4 (425 mg, 2.00 mmol), N-methylbenzylamine (155 μL, 1.20 mmol), iodobenzene (112 μL, 1.00 mmol), ethylene glycol (111 μL, 2.00 mmol) and 1-butanol (1.0 mL) at 90° C. Column chromatography using a solvent mixture (hexane/ethyl acetate=20/1, Rf=0.5) afforded N-methyl-N-phenylbenzylamine (146 mg, 74% isolated yield) as colorless liquid. The spectral data (1H NMR) matched with the literature references and GC analysis indicated >95% purity. See Brenner, E.; Schneider, R.; Fort, Y. Tetrahedron 1999, 55, 12829-12842.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06867298B2 |
| 出典データセット | uspto-grants-2005_03 |
| ORD ID | ord-7684ca4f87274264a6600a8f2a999c66 |
| 出典メモ | uspto-grants-2005_03 |