反应详情

The crude 168A (1.15 g, 6.88 mmol assumed) is dissolved in glacial acetic acid (15 mL) and 2-dimethylamino4-trifluoromethyl-[1,3]oxazin-6-one (1.43 g, 6.88 mmol) is added. The mixture was stirred for 4 h under reflux, after which the acetic acid iss removed in vacuo. The residue is dissolved in ethyl acetate, washed with saturated sodium carbonate solution and water, and is subsequently dried over sodium sulfate. The crude product (1.9 g) is obtained after removal of the drying agent by filtration and evaporation of the solvent. The product (100 mg) is purified by flash chromatography (ethyl acetate/petrol ether 3/7).

1. temperatureunder reflux
2. customafter which the acetic acid iss removed in vacuo
3. dissolutionThe residue is dissolved in ethyl acetate
4. washwashed with saturated sodium carbonate solution and water
5. dry with materialis subsequently dried over sodium sulfate