反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 6-bromo-4-chloro-9-(2-trimethylsilanyl-ethoxymethyl)-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-7-oxide with 6-bromo-2-chloro-9-(2-trimethylsilanyl-ethoxymethyl)-9H-dipyrido[2,3-b;4′,3′-d]pyrrole-7-oxide (4:1, 90 mg, 0.2 mmol), 1,1′-[bis(diphenylphosphino)ferrocene]dichloropalladium(II) (8.5 mg, 0.012 mmol), and triethylamine (0.1 mL, 0.7 mmol) in acetonitrile (1.2 mL) was heated under microwave irradiation at 130° C. for 10 minutes. The cooled reaction mixture was concentrated in vacuo and purified by flash chromatography (silica, 40 g, ISCO, 0-40% ethyl acetate in heptane) to afford the title compound as a 4:1 mixture of the title compound with 6-bromo-2-chloro-9-(2-trimethylsilanyl-ethoxymethyl)-9H-dipyrido[2,3-b;4′,3′-d]pyrrole as an off-white solid (60 mg, 70%). The mixture was used in subsequent steps without any further purification.
WORKUP
后处理
- customThe cooled reaction mixture
- concentrationwas concentrated in vacuo
- custompurified by flash chromatography (silica, 40 g, ISCO, 0-40% ethyl acetate in heptane)