反应详情

温度

50 °C

To a solution of N-(2,6-diisopropyl-3hydroxyphenyl)-2-[4-(3-hydroxypropyl) piperazin-1-yl]acetamide (180 mg, 0.61 mmol) in DMF (3 ml) were added 2-bromoethyl ethyl ether (2 ml) and potassium fluoride catalyst carried on alumina (40 wt %, 355 mg, 2.39 mmol) followed by stirring at 50° C. for 3 hours. After the catalyst was filtered off, the filtrate was diluted with water and extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate and the solvent was evaporated therefrom. The residue was purified by a silica gel column chromatography (developing solvent, chloroform:methanol=20:1) to provide 90 mg (yield 42%) of N-(2,6-diisopropyl-3-(2-ethoxyethyloxy)phenyl)-2-[4-(3-hydroxypropyl)piperazin-1-yl]acetamide as colorless powdery crystals.

1. filtrationAfter the catalyst was filtered off
2. additionthe filtrate was diluted with water
3. extractionextracted with ethyl acetate
4. washThe organic layer was washed with a saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. customthe solvent was evaporated
7. customThe residue was purified by a silica gel column chromatography (developing solvent, chloroform:methanol=20:1)