化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → 5-Bromo-1-(4-fluorophenyl)-3-methyl-1,3-dihydro-benzimidazol-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 5-Bromo-1-(4-fluorophenyl)-1,3-dihydrobenzimidazol-2-one | HCID 59437201 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 5-Bromo-1-(4-fluorophenyl)-3-methyl-1,3-dihydro-benzimidazol-2-one | HCID 59437286 | 95.8% |
反応手順
To a stirred room temperature suspension of 5-bromo-1-(4-fluorophenyl)-1,3-dihydro-benzimidazol-2-one (160 mg, 0.52 mmol) in anhydrous bis(2-methoxyethyl)ether (5 mL) was added lithium bis(trimethylsilyl)amide (0.55 mL of 1.06 M solution in THF, 0.58 mmol). After 30 minutes, methyl iodide (125 μL, 2 mmol) was added. After 2 hours, the mixture was poured into 1 N sulfuric acid containing ice. The resulting precipitate was filtered, washed with water, and dried to afford 160 mg of 5-bromo-1-(4-fluorophenyl)-3-methyl-1,3-dihydro-benzimidazol-2-one as an off-white solid. MS m/z 321/323 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08658637B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-104da1b2cfac47e9a104beb41d3c2052 |
| 出典メモ | uspto-grants-2014_02 |