化工社化工社 化学情報印刷レポート · 研究参考用
Epichlorohydrin → 2-Ethoxy-1-methylpyridinium fluoroborate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Epichlorohydrin | HCID 7835 | — |
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | 1-Methyl-2(1H)-pyridinone | HCID 12755 | — |
| 反応物 | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| 生成物 | 2-Ethoxy-1-methylpyridinium fluoroborate | HCID 13059456 | 71% |
反応手順
Triethyloxonium fluoroborate is prepared from 3.70 g (0.040 mole) of epichlorohydrin in 14 ml of ether and 7.58 g (0.054 mole) of boron trifluoride etherate in 6 ml of ether. The resulting solid triethyloxonium tetrafluoroborate is dissolved in 20 ml of dry methylene chloride and treated under nitrogen with 4.36 g (0.040 mole) of 1-methyl-2-pyridone in 15 ml of methylene chloride. The reaction mixture is stirred under nitrogen at room temperature overnight (about 16 hours). The solvent is evaporated at room temperature, in vacuo and the quaternary salt obtained is recrystallized from methanol-ether (1:1) to give 8.0 g (71%) of 2-ethoxy-1-methylpyridinium fluoroborate, m.p. 58°-60° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04345083 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-184a5348c3a84a9f84afde24a9c1123e |
| 出典メモ | uspto-grants-1982_08 |