反应详情

(3RS,4SR)-4-[4-(2-Chloroethoxy)phenyl]-7-(methoxymethoxy)-3-[4-(methoxymethoxy)phenyl]-3-methylchroman (210 mg, 0.42 mmol) and {(3,5-bis(t-butyl)phenyl]methyl}piperazine (243 mg, 0.84 mmol) were dissolved in a solvent mixture of acetone (4 ml) and DMF (0.4 ml). To the mixture potassium carbonate (116 mg, 0.84 mmol) and tetrabutylammonium iodide (16 mg, 0.04 mmol) added were, and the mixture was stirred while heated under reflux for 3 days. The reaction solution was extracted with ethyl acetate, dried over sodium sulfate, and filtered. The filtrate was evaporated under reduced pressure, and the concentrate thus obtained was subjected to silica gel column chromatography (n-hexane:ethyl acetate=4:1) to give 160 mg (yield: 51%) of a white foamy solid.

1. temperaturewhile heated
2. temperatureunder reflux for 3 days
3. extractionThe reaction solution was extracted with ethyl acetate
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customThe filtrate was evaporated under reduced pressure
7. concentrationthe concentrate thus
8. customobtained