化工社化工社 化学情報印刷レポート · 研究参考用
Potassium Carbonate → (Z)-methyl-3-(2-(3,5-difluorophenoxy)acetamido)but-2-enoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3,5-Difluorophenol | HCID 75928 | — |
| 反応物 | Methyl 3-(2-bromoacetamido)crotonate | HCID 90023822 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | (Z)-methyl-3-(2-(3,5-difluorophenoxy)acetamido)but-2-enoate | HCID 90023395 | 83% |
反応手順
To a suspension of K2CO3 (1.38 g, 10.0 mmol) in acetone (50 mL) were added 3,5-difluorophenol (0.78 g, 6.00 mmol) and (Z)-methyl-3-(2-bromoacetamido)but-2-enoate (1.18 g, 5.00 mmol) and the mixture was refluxed for 5 h. The mixture was cooled to rt and filtered and the filtrate was concentrated in vacuo. To the residue was added DCM (100 mL) and the mixture was washed with water (100 mL×2) and brine (100 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=5:1) to give the title compound as a white solid (1.18 g, 83%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434695B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-e13f3a43cf4f456b92452b03e1590cab |
| 出典メモ | uspto-grants-2016_09 |