関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromonaphthalene | HCID 11372 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1,2-Diaminocyclohexane, trans- | HCID 43806 | — |
| 反応物 | 1-(Pyridin-3-yl)imidazolidin-2-one | HCID 14834204 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Naphthalen-2-yl-3-pyridin-3-ylimidazolidin-2-one | HCID 49872933 | 28% |
反応手順
Copper iodide (10.0 mg, 0.113 mmol), trans-1,2-diamino cyclohexane (10.0 mg, 0.091 mmol) and potassium carbonate (169 mg, 1.22 mmol) were added to a solution of 1,4-dioxane (5 mL) previously purged with argon (10 minutes). The reaction mixture was purged with argon for 10 minutes, followed by the addition of 1-pyridin-3-yl-imidazolidin-2-one (I-1b: 100 mg, 0.61 mmol) and 2-bromo naphthalene (126 mg, 0.61 mmol). The reaction mixture was heated to reflux at 110° C. for 15 hours. The reaction was monitored by TLC (10% MeOH in chloroform). The reaction mixture was filtered through a celite bed and the bed was washed with chloroform. The organic layer was concentrated and purification by column chromatography (using silica gel of mesh size of 60-120, 20% ethyl acetate in hexane as eluent) afforded 48 mg (28% yield) of 1-naphthalen-2-yl-3-pyridin-3-yl-imidazolidin-2-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08263635B2 |
|---|
| 出典データセット | uspto-grants-2012_09 |
|---|
| ORD ID | ord-46f0454602e44c8292f71436466ef06d |
|---|
| 出典メモ | uspto-grants-2012_09 |
|---|