反应详情

Into a 100-mL round-bottom flask, was placed a solution of 4-bromo-3-(2,2,2-trifluoroethyl)benzaldehyde (700 mg, 2.62 mmol, 1.00 equiv) in ethanol:H2O (20:5 mL), NH2OH. hydrogen chloride (235 mg, 3.41 mmol, 1.30 equiv), NaOAc (279 mg, 3.40 mmol, 1.30 equiv). The resulting solution was stirred overnight at room temperature. The reaction was then quenched by the addition of 10 mL of water. The resulting solution was extracted with 3×20 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2×20 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. This resulted in 700 mg (crude) of N-[[4-bromo-3-(2,2,2-trifluoroethyl)phenyl]methylidene]hydroxylamine as yellow oil.

1. customInto a 100-mL round-bottom flask, was placed
2. customThe reaction was then quenched by the addition of 10 mL of water
3. extractionThe resulting solution was extracted with 3×20 mL of ethyl acetate
4. washThe resulting mixture was washed with 2×20 mL of brine
5. dry with materialThe mixture was dried over anhydrous sodium sulfate
6. concentrationconcentrated under vacuum
7. customThis resulted in 700 mg (crude) of N-[[4-bromo-3-(2,2,2-trifluoroethyl)phenyl]methylidene]hydroxylamine as yellow oil