反应详情

570 mg (15 mmol) lithium aluminium hydride are suspended in 150 ml dry THF at RT. 4-[4-(3-Chloro-4-fluoro-phenylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl]-benzoic acid ethyl ester (1.23 g, 3 mmol) are added and the resulting mixture is 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 and the solvent evaporated. The residue was suspended in water, filtered and dried to give the title compound; m.p.>300° C.; HPLC tR=9.14 min.

1. temperaturethe resulting mixture is 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. customthe solvent evaporated
7. filtrationfiltered
8. customdried