関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Methylimidazole | HCID 1390 | — |
| 反応物 | 1,1-Dibromodecane | HCID 11087877 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | Bromodecyl(methylimidazolium)hydrobromide | HCID 67395248 | 68% |
反応手順
A dry 250 mL Schlenk flask was equipped with a magnetic stir bar, dropping funnel, and sealed with a rubber septum. Dibromodecane (73.0 g, 0.24 mol) was dissolved in acetone (50 ml) and added to the flask. The mixture was heated to 55° C. in an oil bath, and 1-methylimidazole (4.0 g, 48.7 mmol) was added over 90 minutes via dropping funnel through the top of the flask under nitrogen flow. After addition, the reaction was allowed to stir at 55° C. for 6 hours. The reaction was cooled and solvent was removed in vacuo. The residue was diluted with 150 mL of hexanes and 60 mL of ethyl acetate and placed in a separatory funnel. The bottom layer was removed and purified by column chromatography over silica (dichloromethane/methanol, 9:1 v/v). Yield: 68%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09181364B2 |
|---|
| 出典データセット | uspto-grants-2015_11 |
|---|
| ORD ID | ord-4f1ff46efd1f447ebac12335f02bb8cb |
|---|
| 出典メモ | uspto-grants-2015_11 |
|---|