反应详情

温度

60 °C

A solution of sodium t-butoxide (49 mg, 0.51 mmol) and (1S,5S)-benzyl 3,6-diazabicyclo[3.2.0]heptane-3-carboxylate (98 mg, 0.24 mmol) in toluene (3 mL) was stirred under nitrogen. To this was added tri-t-butylphosphine (25 mg, 0.05 mmol), palladium (II) acetate (6.9 mg, 0.03 mmol) and 8-iodo-3-(phenylsulfonyl)quinoline (80 mg, 0.202 mmol). The mixture was then heated at 60° C. for 2 h before partitioning between CH2Cl2 and water. The mixture was filtered through Celite and the organic phase was separated. The water phase was extracted twice with CH2Cl2 and the combined extracts dried (Na2SO4), filtered and concentrated in vacuo to provide the crude material, which was purified by flash chromatography to give the title compound.

1. custombefore partitioning between CH2Cl2 and water
2. filtrationThe mixture was filtered through Celite
3. customthe organic phase was separated
4. extractionThe water phase was extracted twice with CH2Cl2
5. dry with materialthe combined extracts dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customto provide the crude material, which
9. customwas purified by flash chromatography