化工社化工社 化学情報印刷レポート · 研究参考用
Diethyl Ether → 3-tert-Butoxy-5-fluoropyrazine-2-carboxaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 3-Tert-butoxy-5-chloropyrazine-2-carboxaldehyde | HCID 22248202 | — |
| 触媒 | Tetraphenylphosphonium Bromide | HCID 2724163 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-tert-Butoxy-5-fluoropyrazine-2-carboxaldehyde | HCID 22248252 | 3.4% |
反応手順
After dissolving 5.86 g of the crude 3-tert-butoxy-5-chloropyrazine-2-carboxaldehyde in 55 ml of acetonitrile, 4.77 g of potassium fluoride, 1.13 g of tetraphenylphosphonium bromide and 0.71 g of 18-crown-6 were added and the mixture was heated to reflux for 4 hours. Diethyl ether was added to the reaction mixture, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. Ethyl acetate was added to the residue, the insoluble portion was filtered out, and the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (solvent: toluene/ethyl acetate) to obtain the title compound (183 mg, 3% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06995144B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-5bb49986b50d4aa78b351e6e7763ddc7 |
| 出典メモ | uspto-grants-2006_02 |