反应详情

A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (150 mg, 0.578 mmol), [3-(1H-1,2,4-triazol-1-yl)phenyl]methylamine (110 mg, 0.636 mmol), Pd2(dba)3 (53 mg, 0.0578 mmol), rac-BINAP (108 mg, 0.173 mmol) and NaOtBu (246 mg, 2.560 mmol) in DMA (5 mL) was heated at 85° C. for 45 minutes. The mixture was allowed to cool, diluted with EtOAc and washed with water. The organic layer was washed with sat.aq. NaHCO3, brine and dried (Na2SO4). Chromatography on silica (EtOAc/hexanes) afforded 4-chloro-6-(2-[1,2,4]triazol-1-yl-benzylamino)-2H-phthalazin-1-one (24 mg) as a yellow solid, 1H (400 MHz, d6-DMSO) δ: 4.54 (d, 2H), 6.86 (s, 1H), 7.18 (dd, 1H), 7.43 (d, 1H), 7.54 (t, 1H), 7.76 (m, 2H), 7.91 (s, 1H), 7.94 (d, 1H), 8.22 (s, 1H), 9.28 (s, 1H), 12.35 (s, 1H) ppm; m/z (M+1) 352.88.

1. temperatureto cool
2. washwashed with water
3. washThe organic layer was washed with sat.aq
4. dry with materialNaHCO3, brine and dried (Na2SO4)