関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Malonate | HCID 7761 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2,3-Difluoropyridine | HCID 2783176 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Diethyl (3-fluoro-2-pyridyl)malonate | HCID 57950221 | 72.8% |
反応手順
A mixture of 3.95 g of 2,3-difluoropyridine, 13.2 g of diethyl malonate, 38 ml of dimethyl sulfoxide and 26.85 g of cesium carbonate was stirred for 3 hours at 100° C. under a nitrogen atmosphere. The reaction mixture was allowed to cool to room temperature, then, to this was added ice water and extracted with ethyl acetate. The organic layer was washed with saturated brine twice, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure. 12.18 g of the resultant residue was subjected to silica gel column chromatography, to obtain 6.38 g of diethyl (3-fluoro-2-pyridyl)malonate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08598176B2 |
|---|
| 出典データセット | uspto-grants-2013_12 |
|---|
| ORD ID | ord-cc1c08c2be1c40b89d03118e493c9979 |
|---|
| 出典メモ | uspto-grants-2013_12 |
|---|