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Ammonia → (3-Benzylphenyl)thiourea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | 3-Benzylaniline | HCID 308869 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | (3-Benzylphenyl)thiourea | HCID 5277306 | — |
反応手順
A solution of 3-benzylaniline (183 mg, 1 mmol) and 1,1′-thiocarbonyldiimidazole (197 mg, 1.1 mmol) in dichloromethane (5 ml) is stirred at room temperature for 1.5 hours. 2 M ammonia in methanol (2.5 ml) is added to the solution and the mixture is stirred at room temperature overnight. The solution is diluted with ethylacetate, and the organic layer is washed with 5% HCl, saturated NaHCO3, and brine, and dried (anhydrous Na2SO4). The crude product is recrystallized from ethylacetate and petroleum ether to give the desired product as a white powder. 1H NMR (300 Hz, CDCl3) δ 7.93 (br s, 1H, NH), 7.73-7.02 (m, 9H, Aryl H), 6.06 (br s, 2H, NH2), 3.98 (s, 2H, CH2). MS (APCI) m/z 243 [M+H]±.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07718671B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-d3a02f982036425fb54709afc3e41d80 |
| 出典メモ | uspto-grants-2010_05 |