化工社化工社 化学情報印刷レポート · 研究参考用
3-Bromopyridine → 3-Benzothiazol-6-yl-1-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Bromopyridine | HCID 12286 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 1-N,2-N-dimethylcyclohexane-1,2-diamine | HCID 551074 | — |
| 反応物 | 1-Benzothiazol-6-yl-5-trifluoromethyl-imidazolidin-2-one | HCID 59636203 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-Benzothiazol-6-yl-1-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one | HCID 49872558 | 45.2% |
反応手順
Using the same reaction conditions and work up as described in Example 1, step-3,1-benzothiazol-6-yl-5-trifluoromethyl-imidazolidin-2-one (I-172b: 0.1 g, 0.0004 mol) was refluxed with 3-bromo-pyridine (0.085 g, 0.0005 mol), copper iodide (0.0076 g, 0.00004 mol), N,N′-dimethyl-cyclohexane-1,2-diamine (0.017 g, 0.00012 mol), potassium phosphate (0.22 g, 0.0012 mol) and 1,4-dioxane (20 mL) at 120° C. for 12 hours to afford the crude product. The reaction was monitored by TLC (100% ethyl acetate). Purification by column chromatography on silica gel (2% methanol in DCM) afforded 54 mg of the product (45.2% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE045173E1 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-dc31d96234044d42853fa7bc593206eb |
| 出典メモ | uspto-grants-2014_09 |