反应详情

温度

150 °C

8.37 g (36.21 mmol) de N-(3-acetylphenyl)-2,2,2-trifluoro-acetamide were dissolved in 80 ml of N,N-dimethyl formamide. To the resultant solution 24.23 ml (181.02 mmol) of N,N-dimethylformamide dimethyl acetal were added and heated at 150° C. for 2 h. The solvent was removed by reduced pressure distillation to yield an oil which was treated with 50 ml of water and extract with 3×100 ml of dichloromethane. The organic layers were washed with 2×200 ml of a saturated solution of sodium chloride, dried over anhydrous sodium sulfate and evaporated to dryness by reduced pressure distillation. A solid was obtained, which precipitated from a mixture of ethanol-ethyl ether to give 4.1 g (yield=55%) of 3-(dimethylamino)-1-[3-(methylamino)phenyl]prop-2-en-1-one.

1. customThe solvent was removed by reduced pressure distillation
2. customto yield an oil which
3. extractionextract with 3×100 ml of dichloromethane
4. washThe organic layers were washed with 2×200 ml of a saturated solution of sodium chloride
5. dry with materialdried over anhydrous sodium sulfate
6. customevaporated to dryness by reduced pressure distillation
7. customA solid was obtained
8. customwhich precipitated from a mixture of ethanol-ethyl ether