反应详情

温度

60 °C

To a solution of 1,4-dichloro-6,7-dihydro-5H-cyclopenta[d]pyridazine (compound 39, 500 mg, 2.64 mmol) in THF (5 mL) is added Pd(PPh3)4 (383 mg, 0.33 mmol). The mixture is degassed and benzyl zinc bromide (11 mL, 0.5 M in THF, 5.6 mmol) is added. The mixture is heated at 60° C. for 5 h. The reaction mixture is cooled down to RT and saturated aq. NaHCO3 solution is added and the mixture is extracted with EtOAc. The combined orgaqnic layers are washed with water, brine, dried over NaSO4, filtered and concentrated. The crude product is purified by flash chromatography (EtOAc/heptane 10%-30%) to give compound 44 (490 mg, 76%).

1. customThe mixture is degassed
2. temperatureThe reaction mixture is cooled down to RT
3. extractionthe mixture is extracted with EtOAc
4. washThe combined orgaqnic layers are washed with water, brine
5. dry with materialdried over NaSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product is purified by flash chromatography (EtOAc/heptane 10%-30%)