反应详情

To the solution of (5-cyano-2-fluorophenyl)boronic acid (660 mg, 4 mmol) in dioxane/H2O (40 mL/13.3 mL) was added phenylmethyl (2S)-4-[(3-bromophenyl)methyl]-2-methyl-1-piperazinecarboxylate (1.2 g, 4 mmol), K2CO3 (2.2 g mg, 16 mmol) and Pd(PPh3)4 (230 mg, 0.2 mmol). The resulting solution was irradiated in a microwave reactor at 150° C. for 20 minutes then diluted with EtOAc (5 mL). The organic layer was collected and the aqueous layer was extracted with EtOAc (2×5 mL). The organic layers were combined, dried over Na2SO4, filtered and concentrated. The residue was purified by Gilson HPLC, eluting with acetonitrile/water/0.1% TFA (10/90 to 90/10, v/v, over 12 min), to give the title compound (708 mg, 92%). LC/MS: m/z, 444 (M+H), 1.93 min.

1. customThe resulting solution was irradiated in a microwave reactor at 150° C. for 20 minutes
2. customThe organic layer was collected
3. extractionthe aqueous layer was extracted with EtOAc (2×5 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by Gilson HPLC
8. washeluting with acetonitrile/water/0.1% TFA (10/90 to 90/10