反应详情

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.

1. concentrationThe reaction mixture is concentrated under reduced pressure and to the obtained residue
2. additionis added 20 ml of ethanol
3. additionAfter the addition of 0.94 g of cyclopropylamine with ice-
4. temperaturecooling
5. concentrationThe reaction mixture is concentrated under reduced pressure
6. customthe obtained residue is purified by chromatography on silica gel