反应详情

5.0 g (12 mMol) of 4-[4-(6-methoxy-pyridin-3-ylmethylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid ethyl ester in 200 ml of THF is cooled to −10° C. Then 80 ml of a 1 N solution of di-isobutyl-aluminium hydride in THF are added dropwise. After stirring for 3 h at RT, 200 ml of THF and 100 ml of EtOAc are added, followed by 10 ml of a 10%-solution of NH4Cl in water. After 30 min vigorous stirring, 20 g of Na2SO4 are added, then the mixture is filtered through Celite. Concentration of the filtrate, stirring in methanol and filtration gives the title compound; MS-ES+: (M+H)+=362.

1. filtrationthe mixture is filtered through Celite
2. stirringConcentration of the filtrate, stirring in methanol
3. filtrationfiltration