関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Bromobenzene | HCID 7961 | — |
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Benzylurea | HCID 10853 | — |
| 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 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Benzyl-3-phenylurea | HCID 280363 | 79.1% |
反応手順
A test tube was charged with CuI (20 mg, 0.10 mmol, 0.10 equiv), K3PO4 (425 mg, 2.0 mmol, 2.0 equiv), benzylurea (225 mg, 1.5 mmol, 1.5 equiv), filled with argon. Bromobenzene (105 μL, 1.0 mmol, 1.0 equiv), N,N′-dimethylethylendiamine (22 μL, 0.20 mmol, 0.20 equiv) and dry dioxane (1.0 mL) were added under argon. The test tube was sealed and the reaction mixture was stirred at 80° C. for 25 h. The resulting suspension was cooled to room temperature and filtered through a 0.5×1 cm pad of silica gel, eluting with ethyl acetate. The filtrate was concentrated in vacuo. The solid residue was dissolved in 2 mL DMF. Purification of the residue by flash chromatography on silica gel (2×20 cm; hexane:ethyl acetate 3:1) provided 179 mg (79% yield) of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06867298B2 |
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| 出典データセット | uspto-grants-2005_03 |
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| ORD ID | ord-993aa8978a1b4b8ab10c1d412c6cf96c |
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| 出典メモ | uspto-grants-2005_03 |
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