関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate | HCID 14652581 | — |
| 生成物 | HCID 178471882 | HCID 178471882 | 89% |
反応手順
4.14 (2H, q, J=7Hz), 7.08-7.52 (1H, m) (2) A solution of 4.46 g of ethyl 4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoylacetate, 1.85 g of dimethylformamide dimethylacetal and 20 ml of toluene is refluxed for 6 hours. The reaction mixture is concentrated under reduced pressure and to the obtained residue is added 20 ml of ethanol. After the addition of 0.94 g of cyclopropylamine with ice-cooling, the mixture is stirred at room temperature for 3 hours. The reaction mixture is concentrated under reduced pressure and the obtained residue is purified by chromatography on silica gel to give 4.06 g of ethyl 2-[4-[2-(N-ethoxycarbonyl-N-methylaminomethyl)morpholino]-2,3,5-trifluorobenzoyl]-3-cyclopropylaminoacrylate in 89% 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-5d2adfb983854fdca9afe5315a07e008 |
|---|
| 出典メモ | uspto-grants-1989_12 |
|---|