反应详情

To 340 mg (0.83 mMol) 4-[4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid lithium salt in 5 ml of DMF under N2-atmosphere, 0.38 ml (3 mMol) of N-ethylpiperazine and 0.31 ml (95%; 2 mMol) of diethyl-cyanphosphonate are added at 0° C. After 60 min, the suspension is diluted with EtOAc and washed with saturated NaHCO3-solution, water and brine. The aqueous layers are reextracted twice with EtOAc, the organic layers dried (Na2SO4) and concentrated after adding SiO2. The resulting powder is put on top of a chromatography column (SiO2) and the title compound eluted with EtOAc/methanol/NH3conc. 80:20:1; HPLC (conditions see Examples 67-78) tR=10.4 min; MS-ES+: (M+H)+=499.

1. washwashed with saturated NaHCO3-solution, water and brine
2. dry with materialthe organic layers dried (Na2SO4)
3. concentrationconcentrated
4. additionafter adding SiO2
5. washthe title compound eluted with EtOAc/methanol/NH3conc