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Sodium Bicarbonate → Ethyl 4-[2-(dimethylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Ethyl 3-oxo-(2,3,4,5-tetrafluorophenyl)propanoate | HCID 600916 | — |
| 反応物 | Dimethyl-morpholin-2-ylmethyl-amine | HCID 3401489 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Ethyl 4-[2-(dimethylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate | HCID 19834973 | 77% |
反応手順
A suspension of 26.4 g of ethyl 2,3,4,5-tetrafluorobenzoylacetate, 18.7 g of 2-(dimethylaminomethyl)morpholine and 8.4 g sodium hydrogencarbonate in 130 ml of acetonitrile is refluxed for 7 hours. The reaction mixture is concentrated under reduced pressure, to the obtained residue is added 100 ml of chloroform and the solution is washed with water. After drying over anhydrous magnesium sulfate, the chloroform is distilled off under reduced pressure and the residue is purified by chromatography on silica gel to give 29.9 g of ethyl 4-[2-(dimethylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate in 77% yield as an oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04889857 |
| 出典データセット | uspto-grants-1989_12 |
| ORD ID | ord-9eb07e61231a4bf19f253f28f837f3be |
| 出典メモ | uspto-grants-1989_12 |