反应详情

To a solution of 1-(4-bromo-phenyl)-3-aza-bicyclo[3.1.0]hexane-3-carboxylic acid tert-butyl ester (Intermediate I, 250 mg, 0.74 mmol) in anhydrous toluene (5 mL) were added Pd2(dba)3 (1.65 mg, 0.002 mmol), BINAP (3.42 mg, 0.006 mmol), sodium tert-butoxide (106.56 mg, 1.11 mmol) and 4-ethyl-[1,4]diazepan-5-one (210.2 mg, 1.48 mmol, prepared by the procedure as described in WO2008136754) at r.t. and reaction mixture was refluxed for 3 h. Reaction mixture was then concentrated and the crude product was purified by column chromatography (silica gel, 0.3:9.7 MeOH:CHCl3) to afford the title compound as viscous liquid (60 mg, 20.3%).

1. customprepared by the procedure
2. customat r.t.
3. customreaction mixture
4. temperaturewas refluxed for 3 h
5. customReaction mixture
6. concentrationwas then concentrated
7. customthe crude product was purified by column chromatography (silica gel, 0.3:9.7 MeOH:CHCl3)