反应详情

温度

90 °C

To a solution of 4-(4,6-dichloro-[1,3,5]triazin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (167.1 mg, 0.5 mmol) in anhydrous 1,4-dioxane (4 mL) in an oven-dried flask was added 3-thiopheneboronic acid (70.4 mg, 0.55 mmol), Pd[P(t-Bu)3]2 (2.5 mg, 0.005 mmol), tris(dibenzylideneacetone)-dipalladium(0) (2.3 mg, 0.0025 mmol), and KF (64 mg, 1.1 mmol). The resulting mixture was vacuum flushed with argon and heated overnight at 90° C. The reaction mixture was cooled and passed through a pad of diatomaceous earth, washing with EtOAc. The filtrate was concentrated and the residue was purified by preparative TLC (EtOAc/hexanes, 1:4) to yield a white solid, which was used without further purification.

1. customflushed with argon
2. temperatureThe reaction mixture was cooled
3. washwashing with EtOAc
4. concentrationThe filtrate was concentrated
5. customthe residue was purified by preparative TLC (EtOAc/hexanes, 1:4)
6. customto yield a white solid, which
7. customwas used without further purification