関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl vinyl ether | HCID 8023 | — |
| 反応物 | 4-Iodopyrazole | HCID 77022 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 1-(1-Ethoxyethyl)-4-iodo-1H-pyrazole | HCID 4640409 | 73% |
反応手順
4-Iodo-1H-pyrazole (3.0 g) was suspended in benzene (150 mL) and the suspension was heated while stirring. Ethyl vinyl ether (4.4 mL) was added thereto, concentrated HCl was added dropwise thereto, and the resulting mixture was stirred at 60° C. for 3 hours. After completion of the reaction, the resulting mixture was concentrated by evaporation under a reduced pressure, and the residue was neutralized using aqueous saturated sodium hydrogen carbonate (10 mL). The resulting mixture was extracted with ethyl acetate (50 mL) and the extract was washed successively with distilled water (100 mL). The organic layer was dried over anhydrous magnesium sulfate and concentrated by evaporation under a reduced pressure. The resulting residue was purified by silica gel chromatography to obtain the title compound as a transparent yellow liquid (3.0 g, yield 73%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08063229B2 |
|---|
| 出典データセット | uspto-grants-2011_11 |
|---|
| ORD ID | ord-94e6445547334ae2a15fb757df2d980c |
|---|
| 出典メモ | uspto-grants-2011_11 |
|---|