反应详情

The mixture of 4-(2,2,2-Trifluoro-ethoxy)-phenylamine (2.5 g, 13 mmol), 4-bromobut-1-ene (3.54 g, 26 mmol) and Cs2CO3 (6.41 g, 20 mmol) was stirred in 30 mL of DMF at ambient temperature for 72 h. And then the mixture was filtered and washed with water. The filtrate was extracted with EtOAc (30 mL×3). The combined organic layers was washed with brine and dried with anhydrous sodium sulfate and evaporated to dryness. The residue was purified by silica-gel column chromatography (eluting with petroleum ether/ethyl acetate=30:1). The title compound (0.7 g, 22%) as brown oil was obtained. LC-MS: 246.1 [M+1]+.

1. filtrationAnd then the mixture was filtered
2. washwashed with water
3. extractionThe filtrate was extracted with EtOAc (30 mL×3)
4. washThe combined organic layers was washed with brine
5. dry with materialdried with anhydrous sodium sulfate
6. customevaporated to dryness
7. customThe residue was purified by silica-gel column chromatography (eluting with petroleum ether/ethyl acetate=30:1)