化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Diaminocyclohexane → 1-Benzothiazol-6-yl-3-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Diaminocyclohexane | HCID 4610 | — |
| 反応物 | 3-Bromopyridine | HCID 12286 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 1-Benzothiazol-6-yl-4-trifluoromethyl-imidazolidin-2-one | HCID 68787913 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Benzothiazol-6-yl-3-pyridin-3-yl-4-trifluoromethyl-imidazolidin-2-one | HCID 49872649 | 23.8% |
反応手順
Using the same reaction conditions and work up as described in example 1, step-3,1-Benzothiazol-6-yl-4-trifluoromethyl-imidazolidin-2-one (I-170b: 50 mg, 0.174 mmol) was refluxed with 3-Bromo-pyridine (33 mg, 0.209 mmol), copper iodide (3.3 mg, 0.0174 mmol), Cyclohexane-1,2-diamine (6 mg, 0.0522 mmol), potassium phosphate (110 mg, 0.522 mmol) and 1,4-Dioxane (2 mL) at 120° C. for 12 hours to afford the crude product. Purification by column chromatography on silica gel (2% methanol in chloroform) followed by n-pentane washing afforded 15 mg of the product (23.8% 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-10082d1ae133471d889e5801d44f73b2 |
| 出典メモ | uspto-grants-2014_09 |