反应详情

After 3.055 g (8.403 mmol) of 1-benzyl-3-(2-tert-butyldimethylsiloxy-1-hydroxyethyl)-4-piperidinone was dissolved in 100 ml of methanol, 10 ml of concentrated hydrochloric acid was added, followed by stirring at room temperature for 10 minutes. The solvent was distilled off under reduced pressure with heating. The resulting residue was dissolved in water. After this solution was alkalified with aqueous sodium hydroxide, it was extracted with dichloromethane 3 times. The combined organic layer was dried over anhydrous magnesium sulfate; the solvent was distilled off under reduced pressure. The resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1 to 6/1) to yield 5-benzyl-4,5,6,7-tetrahydrofuro[3,2-c]pyridine.

1. distillationThe solvent was distilled off under reduced pressure
2. temperaturewith heating
3. dissolutionThe resulting residue was dissolved in water
4. extractionwas extracted with dichloromethane 3 times
5. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe resulting crude product was purified by silica gel column chromatography (hexane/ethyl acetate=9/1 to 6/1)