HRID60317

反应详情

EQUATION

反应方程式

HRID 60317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe cooled reaction mixture
  2. concentrationwas concentrated in vacuo
  3. custompurified by flash chromatography (silica, 40 g, ISCO, 0-40% ethyl acetate in heptane)