反应详情

温度

100 °C

To a sealed tube under nitrogen was added 1-((6-chloropyridin-3-ylmethyl)-4-methylpiperazine (13.5 g, 59.8 mmol, Eq:1.00), 2-(dicyclohexylphosphino)biphenyl (4.19 g, 12.0 mmol, Eq:0.20), tris(dibenzylideneacetone)-dipalladium (0) (5.48 g, 5.98 mmol, Eq: 0.10), and lithium bis(trimethylsilyl)amide, 150 ml of a 1.0M solution in THF. An additional 150 ml THF was added. The flask was degassed with argon. The flask was capped and the reaction heated at 100° C. overnight. 3M HCl was added along with DCM to the material and the layers were separated. The aqueous layer was bacidified with 3M NaOH. The aqueous layer was then extracted 3 times with DCM to provide 3.2 g (25.9%) of a yellow powder which was used without further purification.

1. customThe flask was degassed with argon
2. customThe flask was capped
3. addition3M HCl was added along with DCM to the material
4. customthe layers were separated
5. extractionThe aqueous layer was then extracted 3 times with DCM