反应详情

Under nitrogen atmosphere a solution of dimethylzinc in toluene (1.2 M, 19.1 mL) is added to a mixture of 6-bromo-pyrrolo[2,1-b]thiazole-7-carboxylic acid ethyl ester (11.4 mmol) and [1,1′-Bis(diphenylphosphino)ferrocene]dichloropalladium(II) (0.23 mmol, complex with CH2Cl2) in dioxane (35 mL). The mixture is heated to reflux for 2 h, stirred at RT for 12 h and diluted by addition of MeOH (2.3 mL) and TBME. The mixture is washed with hydrochloric acid (1.0 M) and water, dried over MgSO4, concentrated in vacuo and purified by flash chromatography (gradient: heptane to heptane/EtOAc 8/2) to give the desired product. LC-MS: tR=0.91 min; [M+H]+=210.0.

1. temperatureThe mixture is heated
2. temperatureto reflux for 2 h
3. washThe mixture is washed with hydrochloric acid (1.0 M) and water
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. custompurified by flash chromatography (gradient: heptane to heptane/EtOAc 8/2)