反应详情

A mixture 6-bromo-4-chloro-2H-phthalazin-1-one (145 mg, 0.559 mmol), 1-(2-pyrazinyl)piperazine (104 mg, 0.633 mmol), Pd2(dba)3 (43 mg, 0.047 mmol), rac-BINAP (116 mg, 0.186 mmol) and NaOtBu (167 mg, 1.738 mmol) in DMA (5 mL) was heated at 85° C. for 1.5 h. 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). Preparatory HPLC afforded 4-chloro-6-(2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-yl)-2H-phthalazin-1-one (32 mg) as a yellow solid, 1H (400 MHz, d6-DMSO) δ: 3.62 (m, 4H), 3.78 (m, 4H), 7.12 (d, 1H), 7.60 (dd, 1H), 7.87 (d, 1H), 8.07 (d, 1H), 8.11 (m, 1H), 8.37 (s, 1H), 12.51 (s, 1H) ppm. m/z (M+1) 342.98.

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