反应详情

570 mg (15 mmol) lithium aluminum hydride are suspended in 150 ml dry THF at RT. 1.23 g (3 mmol) 4-[4-((R)-1-phenyl-ethylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid ethyl ester are added and the mixture heated to reflux for 1 h. The mixture is cooled in an ice bath and treated sequentially with water (0.57 ml), 15% sodium hydroxide solution (0.57 ml) and water (1.71 ml). The solid aluminum complex is removed by filtration (Hyflo Super Cel®; Fluka, Buchs, Switzerland), the filtrate dried over sodium sulfate evaporated. The residue is suspended in water, filtered and dried to give the title compound; m.p.>300° C.; Rf(dichloromethane/ethanol 9:1 plus 1% conc. ammonia)=0.43; HPLC tR=8.71 min.

1. temperaturethe mixture heated
2. temperatureto reflux for 1 h
3. temperatureThe mixture is cooled in an ice bath
4. customThe solid aluminum complex is removed by filtration (Hyflo Super Cel®; Fluka, Buchs, Switzerland)
5. dry with materialthe filtrate dried over sodium sulfate
6. customevaporated
7. filtrationfiltered
8. customdried