反应详情

1.56 ml of diisobutyl-aluminium hydride (1 M in THF) are added to a solution of 130 mg (0.26 mMol) of (4-ethyl-piperazin-1-yl)-{4-[4-(4-fluoro-2-methyl-1H-indol-5-yloxy)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-phenyl}-methanone in 13 ml of THF at −15° C. under a N2-atmosphere. After 3 h, 4 ml of EtOAc are added to the solution, followed by 0.2 ml of a saturated solution of NH4Cl in water. After adding solid Na2SO4, the reaction mixture is filtered through Celite. The filtrate is concentrated together with 3 g of SiO2. The resulting powder is put on top of a chromatography column (SiO2) and then eluted with EtOAc/methanol 4:1 and finally EtOAc/methanol/NEt3 80:20:1, yielding the title compound; HPLC (conditions see Examples 67-78) tR=10.5 min; MS-ES+: (M+H)+=485.

1. filtrationthe reaction mixture is filtered through Celite
2. concentrationThe filtrate is concentrated together with 3 g of SiO2
3. washeluted with EtOAc/methanol 4:1 and finally EtOAc/methanol/NEt3 80:20:1