反应详情

To a solution of 1-Boc-azetidin-3-on (240 mg) in methanol (20 ml) were added methylamine hydrochloride (1.42 g) and 10% palladium carbon (1.0 g), followed by stirring under hydrogen atmosphere at room temperature for 60 hours. The reaction mixture was filtered to remove the catalyst. To the filtrate was added again 10% palladium carbon (1.0 g), followed by stirring under hydrogen atmosphere (0.40 MPa) at room temperature for 9 hours. The reaction mixture was filtered to remove the catalyst, and the filtrate was concentrated under reduced pressure. To the resultant residue were added a saturated aqueous solution of sodium hydrogencarbonate, ethyl acetate and potassium carbonate, followed by partition. The aqueous layer was extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate, concentrated under reduced pressure to provide a crude product of the title compound (216 mg) as a pale yellow oil.

1. filtrationThe reaction mixture was filtered
2. customto remove the catalyst
3. additionTo the filtrate was added again 10% palladium carbon (1.0 g)
4. stirringby stirring under hydrogen atmosphere (0.40 MPa) at room temperature for 9 hours
5. filtrationThe reaction mixture was filtered
6. customto remove the catalyst
7. concentrationthe filtrate was concentrated under reduced pressure
8. additionTo the resultant residue were added a saturated aqueous solution of sodium hydrogencarbonate, ethyl acetate and potassium carbonate
9. customby partition
10. extractionThe aqueous layer was extracted with ethyl acetate
11. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
12. concentrationconcentrated under reduced pressure