反应详情

A solution of ethyl 2-chloro-4-morpholino-5H-pyrrolo[3,4-d]pyrimidine-6(7H)-carboxylate (intermediate 27) (156 mg, 0.498 mmol), 1-ethyl-3-(3-fluoro-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)urea (intermediate 28) (174 mg, 0.567 mmol), [1,1′-Bis (diphenylphosphino)ferrocene]dichloropalladium (II), complex with dichloromethane (20 mg, 0.0249 mmol) and sodium carbonate (148 mg, 1.39 mmol) in 2 ml of a 7:3:1 mixture of DME:H2O:EtOH respectively was heated in the microwave at 115° C. for 45 minutes. The reaction was concentrated in vacuo and the residue re-dissolved in a mix of MeOH/DCM. It was loaded onto an SCX cartridge and washed with two column volumes of MeOH/DCM before being eluted with 2M NH3 in MeOH and concentrated in vacuo to give a solid. The solid was triturated in acetone and filtered to yield the title compound (45 mg, 20%).

1. concentrationThe reaction was concentrated in vacuo
2. dissolutionthe residue re-dissolved in
3. additiona mix of MeOH/DCM
4. washwashed with two column volumes of MeOH/DCM
5. washbefore being eluted with 2M NH3 in MeOH
6. concentrationconcentrated in vacuo
7. customto give a solid
8. customThe solid was triturated in acetone
9. filtrationfiltered