化工社化工社 化学情報印刷レポート · 研究参考用
HRID 253221作成日:2026年10月27日
3,4-Dimethoxybenzeneacetonitrile → 2-[3,4-Bis(methyloxy)phenyl]-3-oxo-4-(2-oxopyrrolidin-1-yl)butanenitrile
https://huagongshe.com/reaction/253221
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3,4-Dimethoxybenzeneacetonitrile | HCID 66727 | — |
| 反応物 | Methyl 2-oxo-1-pyrrolidineacetate | HCID 108835 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[3,4-Bis(methyloxy)phenyl]-3-oxo-4-(2-oxopyrrolidin-1-yl)butanenitrile | HCID 66891041 | 25.5% |
反応手順
To a mixture of [3,4-bis(methyloxy)phenyl]acetonitrile (1.0 g, 5.5 mmol) and methyl (2-oxopyrrolidin-1-yl)acetate (1.0 g, 7.0 mmol) in ethanol (4 mL) was added a sodium ethoxide solution (21%, 4.2 mL, 11 mmol), and the resulting mixture was heated at reflux for 18 hours. After cooling to room temperature, it was poured into a mixture of ice-water (50 mL). This aqueous mixture was washed with dichloromethane (3×20 mL) then acidified to pH 1. The acidified mixture was extracted with ethyl acetate (3×30 mL). The combined extract was washed with aqueous sodium bicarbonate solution, brine, dried over sodium sulfate, filtered and concentrated to give 2-[3,4-bis(methyloxy)phenyl]-3-oxo-4-(2-oxopyrrolidin-1-yl)butanenitrile as a brown oil (0.43 g, 1.4 mmol, 25% yield), MS (EI) for C16H18N2O4: 303 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07872014B2 |
|---|
| 出典データセット | uspto-grants-2011_01 |
|---|
| ORD ID | ord-808e0f393b3a4a628f7f087ed182a181 |
|---|
| 出典メモ | uspto-grants-2011_01 |
|---|