関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | Butylurea | HCID 11595 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | Benzene, 1-iodo-3-methoxy- | HCID 69839 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-Butyl-3-(3-methoxyphenyl)urea | HCID 4053589 | 85% |
反応手順
A test tube was charged with CuI (10 mg, 0.05 mmol, 0.05 equiv), K3PO4 (425 mg, 2.0 mmol, 2.0 equiv), butylurea (232 mg, 2.0 mmol, 2.0 equiv), filled with argon. 3-Iodoanisole (119 μL, 1.0 mmol, 1.0 equiv), N,N′-dimethylethylendiamine (11 μL, 0.10 mmol, 0.10 equiv) and dry toluene (1.0 mL) were added under argon. The test tube was sealed and the reaction mixture was stirred at 110° C. for 24 h. The resulting suspension was cooled to room temperature and filtered through a 0.5×1 cm pad of silica gel, eluting with diethyl ether. The filtrate was concentrated in vacuo. Purification of the residue by flash chromatography on silica gel (2×20 cm; pentane:diethyl ether 1:2) provided 188 mg (85% yield) of the title compound as a light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07115784B2 |
|---|
| 出典データセット | uspto-grants-2006_10 |
|---|
| ORD ID | ord-30b481f6305e4b7e8c9bbcc591d90100 |
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| 出典メモ | uspto-grants-2006_10 |
|---|
