反应详情

To the mixture of but-3-enyl-[4-(2,2,2-trifluoro-ethoxy)-phenyl]-amine (1.56 g, 6 mmol) and NEt3 (1.7 g, 17 mmol) in 30 mL of DCM, acryloyl chloride (0.65 g, 7 mmol) was added slowly into at 0° C. The mixture was stirred at ambient temperature overnight. And then the solution was washed with water (2×15 mL) and brine (2×20 mL), dried with anhydrous sodium sulfate and evaporated to dryness. The residue was purified by silica-gel column chromatography (eluting with petroleum ether/ethyl acetate=20:1) to obtain the title compound (1.6 g, 89%) as colorless oil. LC-MS: 300.1 [M+1]+.

1. additionwas added slowly into at 0° C
2. washAnd then the solution was washed with water (2×15 mL) and brine (2×20 mL)
3. dry with materialdried with anhydrous sodium sulfate
4. customevaporated to dryness
5. customThe residue was purified by silica-gel column chromatography (eluting with petroleum ether/ethyl acetate=20:1)