反应详情

A mixture of tert-butyl {1-[4-(2-chloro-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]cyclobutyl}carbamate (150 mg, 0.292 mmol), [4-(benzyloxycarbonyl)phenyl]boronic acid (149 mg, 0.584 mmol), bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)dichloropalladium(II) (21 mg, 0.029 mmol), and 2M Na2CO3 aq. (0.292 mL, 0.584 mmol) in DMF (3 mL) was treated with microwave (160° C. for 1 hour). The mixture was diluted with AcOEt, washed with water (×3), brine, dried over Na2SO4, then filtrated through Celite pad. The filtrate was concentrated and the residue was purified by preparative thin-layer chromatography (n-hexane/AcOEt=1:2) to afford the desired product (102 mg, 51%) as a yellow solid. LCMS: 690 [M+H].

1. additionwas treated with microwave (160° C. for 1 hour)
2. washwashed with water (×3), brine
3. dry with materialdried over Na2SO4
4. filtrationfiltrated through Celite pad
5. concentrationThe filtrate was concentrated
6. customthe residue was purified by preparative thin-layer chromatography (n-hexane/AcOEt=1:2)