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Tetrahydrofuran → 3,3',3''-(benzene-1,3,5-triyltris(methylene))tris(4,5-dichloro-1-(naphthalen-2-ylmethyl)-1H-imidazol-3-ium) bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Bromomethylnaphthalene | HCID 70320 | — |
| 反応物 | 4,5-Dichloroimidazole | HCID 140018 | — |
| 反応物 | 1,3,5-Tris(bromomethyl)benzene | HCID 530258 | — |
| 生成物 | 3,3',3''-(benzene-1,3,5-triyltris(methylene))tris(4,5-dichloro-1-(naphthalen-2-ylmethyl)-1H-imidazol-3-ium) bromide | HCID 86719620 | — |
反応手順
4,5-dichloroimidazole (3.00 g, 21.90 mmol) was dissolved in THF and brought to reflux. Potassium hydroxide (2.46 g, 43.80 mmol) was added to the solution and allowed to reflux for 30 min. 1,3,5-tris(bromomethyl)benzene (2.61, 7.30 mmol) was added to the solution and refluxed overnight. Solution was filtered while hot to remove the KBr precipitate and the filtrate returned to reflux. 2-(bromomethyl)naphthalene (4.84 g, 21.90 mmol) was added to the solution and refluxed for 3 h. The volatiles were removed in vacuo and the resulting waxy yellow solid was washed in ethyl ether. A white precipitate was collected and analyzed. 1H NMR (300 MHz, DMSO-d6): δ 4.87, 5.18, 7.32, 7.57, 7.95, 10.30.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09278951B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-ddf15657a63c49be977fa70256857053 |
| 出典メモ | uspto-grants-2016_03 |