反应详情

13.1 g of {4-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-4-oxo-butyl}-methyl-carbamic acid tert-butyl ester (27.66 mmol) were dissolved in 250 ml of tetrahydrofuran. 44.9 g of borane in tetrahydrofuran (522.44 mmol) were added dropwise within 25 min. and then the reaction mixture was heated to reflux for 1.5 h. The reaction mixture was poured onto water and extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and concentrated to dryness. The crude product was purified by chromatography on silica gel using dichloromethane-methanol (0-5%) as eluent. Fractions containing the product were combined and the solvent evaporated to yield 8.2 g of the title compound.

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 1.5 h
3. additionThe reaction mixture was poured onto water
4. extractionextracted with ethyl acetate
5. dry with materialThe organic layer was dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated to dryness
8. customThe crude product was purified by chromatography on silica gel
9. additionFractions containing the product
10. customthe solvent evaporated