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Triethylamine → 2-(Methylthio)-cis-4,5-diphenyl-4,5-dihydro-imidazole-1-carboxylic Acid Phenyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | cis-4,5-Diphenyl-2-methylthio-4,5-dihydro-1H-imidazole hydroiodide | HCID 68569083 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Methylthio)-cis-4,5-diphenyl-4,5-dihydro-imidazole-1-carboxylic Acid Phenyl Ester | HCID 59655459 | 59.2% |
反応手順
To a solution of 2-(methylthio)-cis-4,5-diphenyl-4,5-dihydro-1H-imidazole hydroiodide (42) (1.00 mg, 2.52 mmol), triethylamine (0.528 mL, 0.379 mmol), 4-dimethylamino-pyridine (10 mg) in dichloromethane (20 mL) is added phenyl chloroformate (0.379 mL, 3.02 mmol), and the mixture is stirred at rt overnight. The reaction mixture is diluted with dichloromethane and washed with water, brine, and the organic layer is dried (MgSO4), filtered, and evaporated. The residue is purified by chromatography on silica gel; gradient elution with heptane:EtOAc (70:30-60:40) gives 0.58 g of the product 548. 1H NMR (CDCl3) δ 7.25-6.95 (m, 11H), 6.95-6.80 (m, 2H), 6.80-6.70 (m, 2H), 5.80-5.65 (m, 2H), 2.62 (s, 3H). MS: m/z 389 (M++1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741493B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-38f7a9f155714a62b76115b2a7142ad9 |
| 出典メモ | uspto-grants-2010_06 |