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Dimethylcarbamoyl Chloride → N'-(4-bromo-2-fluorobenzyl)-N,N-dimethylurea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylcarbamoyl Chloride | HCID 6598 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (4-Bromo-2-fluorophenyl)methanamine | HCID 3770848 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N'-(4-bromo-2-fluorobenzyl)-N,N-dimethylurea | HCID 67225137 | — |
反応手順
N,N-Dimethylcarbamoyl chloride (101 μL, 1.1 mmol) was added to a solution of 1-(4-bromo-2-fluorophenyl)methanamine (0.204 g, 1.0 mmol) and triethylamine (148.1 μL, 1.10 mmol) in methylene chloride (5 mL) at 0° C., followed by 4-dimethylaminopyridine (0.012 g, 0.1 mmol). After 10 min, the ice-water bath was removed and the mixture was stirred overnight at RT. The mixture was washed with water and brine. The organic layer was dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue (253 mg, 91.9%) was directly used in next step without further purification. LCMS: (M+H)=276.9/274.9.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07767675B2 |
| 出典データセット | uspto-grants-2010_08 |
| ORD ID | ord-d0bc222f51e94dbab84bdf4c99763d31 |
| 出典メモ | uspto-grants-2010_08 |